X-ray imaging is a very useful plasma diagnostic method. A theoretical analysis of the x-ray phase imaging in the method based on Fresnel diffraction is given. The authors show it is a linear band pass filter, a property suit for Rayleigh-Taylor (R-T) instability measurement. The evaluation permits the possibility of R-T instability measurement in x-ray phase imaging
Structure of ferrite in drawn pearlitic steel containing 0.9 mass% C was investigated with X-raydiffraction technique using synchrotron radiation. In the detailed analysis of diffraction peaks of ferrite during the drawing process, it was experimentally revealed that the transformation of ferrite from bcc to bct due to the supersaturation of carbon in ferrite of heavily drawn pearlitic steel.
Structure of ferrite in drawn pearlitic steel containing 0.9 mass% C was investigated with X-raydiffraction technique using synchrotron radiation. In the detailed analysis of diffraction peaks of ferrite during the drawing process, it was experimentally revealed that the transformation of ferrite from bcc to bct due to the supersaturation of carbon in ferrite of heavily drawn pearlitic steel.
AbstractX-raydiffractionanalysis of pressure-induced structural changes in the Aequorea yellow fluorescent protein Citrine reveals the structural basis for the continuous...Full Text Available
TlGaSe_2 compound belongs to group of layered semiconductors of A"3B"3C_2"6-type. Photoelectric and optical properties of TlGaSe_2 single crystals were investigated in detail. Influence of gamma-, electron and neutron radiation on photoelectric properties of TlGaSe_2 single crystals is investigated too. The present work deals with experimental results relative to X-ray dosimetric characteristics of TlGaSe_2 crystals at 300 K. X-ray conductivity and X-ray dosimetric characteristic measurements are carried out in low load resistance regime. The source of X-ray radiation is the installation of X-raydiffractionanalysis (URS-55a) with the BCV-2(Cu). Intensity of X-ray radiation (E) is regulated by measurement with current variation in tube at each given value of X-ray radiation dose E (R/min) are ...
Oxide superconducting thin films were irradiated with X-rays and ultra-violet (UV) light, and induced radiation effects on electrical and chemical properties were examined by transport measurement, X-raydiffractionanalysis (XRD), diamagnetization measurement and X-ray photoemission spectroscopy (XPS). After irradiation for ErBa_2Cu_3O_x films with X-rays emitted from a Rh tube for 100 hours, superconductivity was remarkably damaged, destroying the zero-resistance state. The UV-light irradiation for Bi_2Sr_2CaCu_2O_x films was performed in He gas of about 500 Pa with a low pressure mercury lamp. The superconductivity was gradually degraded with the UV irradiation time up to 70 minutes. In both cases, adequate oxygen-annealing treatments restored superconductivity. The X-ray photoemission spectra showed that the mean Cu valence of the films ...
The issue of beam-induced damage on diffractive hard X-ray optics is addressed. For this purpose a systematic study on the radiation damage induced by a high-power X-ray beam is carried out in both...Full Text Available
The following are reported: colorimetric determination of Ti in Cr, decontamination of metals by anodic dissolution, computer code for x-ray peak identification, gel-permeation chromatography of CoRezyn 1664 polyester resin, infrared monitoring of gases and vapors, particle size analysis of dusts, nondestructive analysis of Oralloy for removable alpha contamination, dissolution (digestion) of high-fired oxides, assay of U in a Pu-U alloy, measurement of oxide thickness on Pu metal by x-raydiffraction, analysis of precipitated Pu peroxide, differentiation of Dowex SBR and 11 resins, and determination of Pu solubility in simulated lung fluid.
... The constancy of the X-ray intensity ratio for each element in Table 8 as the X-ray tube settings were changed shows the excellent compensating ...
This work analyzes the unoptimized prototype triode-sputtered, 150 microns thick tantalum coatings deposited with a 2.5 microns niobium underlayer on the bore of a large-diameter A723 steel cylinder. The coating was deposited for wear and erosion protection by Pacific Northwest National Laboratory. The phase determination was based on Xraydiffractionanalysis, wavelength dispersive Xray fluorescence analysis, energy dispersive Xrayanalysis, and hardness and electrical resistivity measurements. Both Xraydiffraction and radius-of- curvature methods were used to determine residual stresses. A locally developed high-resolution pole figure technique was used to perform texture analysis. The ...
The use of X-raydiffraction line profile analysis for the study of nanocrystalline powders is described. The fundamentals of the theory are presented in terms of crystallite/domain size, size distribution, lattice distortion, dislocations density and stacking faults. Line profile parameters and the methods of pattern fitting introduced to overcome the diffraction-line overlap problem are discussed. The approaches based of the integral breadth of the measured line profiles and the Fourier method are discussed. In addition, simplified approaches are also commented. Representative examples are selected to illustrate various cases of microstructure, such as nanomaterials with strain-free spherical nano crystallites, strain-free crystallites with anisotropic crystallite shape, anisotropic crystallites with microstrains and spherical crystallites with dislocation densities and crystallite size distributions. ...
This paper presents results about the characterisation of the biomass fly ashes sourced from a thermal power plant and from a co-generation power plant located in Portugal, and the study of new cement formulations incorporated with the biomass fly ashes. The study includes a comparative analysis of the phase formation, setting and mechanical behaviour of the new cement-fly ash formulations based on these biomass fly ashes. Techniques such as X-raydiffraction (XRD), X-ray fluorescence spectroscopy (XRF), thermal gravimetric and differential thermal analysis (TG/DTA), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and environmental scanning electron spectroscopy (ESEM) were used to determine the structure and composition of the formulations. Fly ash F1 from the t...
Chemical phase identifications of complex, multilayered corrosion products formed on Fe-Ni-Cr alloys immersed in molten NaNO/sub 3/-KNO/sub 3/ and LiNO/sub 3/-NaNO/sub 3/-KNO/sub 3/ were obtained by X-raydiffractionanalysis. Diffraction analyses performed after successive material removal steps provided depth profiles of corrosion products and identified the dominant phases as NaFeO/sub 2/, Fe/sub 3/O/sub 4/, and Cr/sub 2/O/sub 3/ for Alloy 800 and 316SS after immersion in NaNO/sub 3/-KNO/sub 3/. In LiNO/sub 3/-NaNO/sub 3/-KNO/sub 3/, the major corrosion products identified on Alloy 800 were LiFeO/sub 2/, Fe/sub 3/O/sub 4/, and Cr/sub 2/O/sub 3/. X-raydiffraction results were supplemented by electron microprobe analyses that revealed the solid solution nature of several of the oxide phases.
The physical properties of polymer blends consisting of one or more crystallizable components are affected by the microstructure of these materials. In particular, the degree of crystallinity can be influenced by processing parameters, and the crystallinity, as well as the phase distribution, may vary as a function of depth through an injection molded part Conventional x-raydiffraction techniques can provide information regarding both phase composition and degree of crystallinity, but, because of the relative transparency of these materials to wavelengths generally available in the laboratory, these techniques provide information representative of only the bulk. By employing parallel beam optics at varying grazing incidence angles, the x-ray sampling depth can be varied without loss of resolution. This technique can be used to vary the effective analysis depth from the top several hundred angstroms for ...
The physical properties of polymer blends consisting of one or more crystallizable components are affected by the microstructure of these materials. In particular, the degree of crystallinity can be influenced by processing parameters, and the crystallinity, as well as the phase distribution, may vary as a function of depth through an injection molded part Conventional x-raydiffraction techniques can provide information regarding both phase composition and degree of crystallinity, but, because of the relative transparency of these materials to wavelengths generally available in the laboratory, these techniques provide information representative of only the bulk. By employing parallel beam optics at varying grazing incidence angles, the x-ray sampling depth can be varied without loss of resolution. This technique can be used to vary the effective analysis depth from the top several hundred angstroms for ...
Fuel irradiation leads to a swelling resulting from the formation of gaseous (Kr, Xe) or solid fission products which are found either in solution or as solid inclusions in the matrix. This phenomena has to be evaluated to be taken into account in fuel cladding Interaction. Fuel swelling was studied as a function of burn up by measuring the corresponding cell constant evolution by X-Raydiffraction. This study was realized on Mixed Oxide Fuels (MOX) irradiated in a Pressurized Water Reactor (PWR) at different burn-up for 3 initial Pu contents. Lattice parameter evolutions were followed as a function of burn-up for the irradiated fuel with and without an annealing thermal treatment. These experimental evolutions are compared to the theoretical evolutions calculated from the hard sphere model, using the fission product concentrations determined by the APPOLO computer code. Contribution of varying parameters influencing the unit cell value is ...
Structural relaxation, crystallization and optimisation processes in soft magnetic amorphous alloys based on iron are examined by applying different experimental techniques: X-raydiffractionanalysis, high-resolution electron microscopy, measurements of magnetic and electric properties (permeability, after-effect resistivity). The presented results are discussed in terms of annealing out of microvoids, formation of nanocrystalline phase and changes of effective magnetostriction constant. (author)
The structural variations of amorphous metals, such as Pd/sub 80/Si/sub 20/, with irradiation of helium ion, neutron, and gamma ray have been mainly pursued by the method of X-raydiffraction and thermal analysis. It should be noticed that the amorphous metals show a radiation resistance, that is, no remarkable structural changes under helium ion, neutron, and gamma ray irradiation.
By means of infrared spectroscopy, x-raydiffraction, and differential thermal analysis, the authors investigate the pyrolysis of dichlorodithiourea cadmium, the vapor phase epitaxy of the cadmium sulfide film, and the composition of the solid and gaseous pyrolysis products. Those products are found to include the thiocyanates of guanidine, ammonium, and hydrogen along with cadmium oxides and sulfates and hydrochloric acid.
Peculiarities of metastable #beta#-solid solution decmposition in titanium alloy VT30 in the process of isothermal ageing in the range 500-650 deg C are investigated. Using the methods of transmittion electron microscopy, X-raydiffractionanalysis, etc., it is shown that in the case of alloy quenching from the temperature below the point of complete polymorphous transformation (T_t_._t_.), as well as after warm rolling the course of subsequent decomposition of solid solution can be consierably complicated.
X-ray scattering methods suitable for the investigation of the morphology and chemical composition of self-organized quantum dots and quantum wires are reviewed. Their application is demonstrated in experimental examples showing that a combination of small angle X-ray scattering with high-resolution X-raydiffraction can reveal both the shape and the chemical composition of the self-organized objects. (author)
A possible novel application of hard x-ray emitted during laser-plasma interaction was discussed. The authors established an Optical Transform Function to study the joint effect of the spectral distribution and temporal profile of the laser-produced x-ray on x-ray phase imaging. Though the laser-produced x-ray pulse duration is short and incoherent, the analysis confirms that the current x-ray phase imaging theory still holds for laser-produced x-ray phase imaging
One aspect of the research program SFB 570 'Distortion engineering' is the in situ X-Raydiffractionanalysis of phases and residual stresses during complete heat treatment cycles. These investigations result in experimental evidence available for the extensive computations. The optimisation of the instrumentation will be reported. A surface decarburisation of samples made from the ball bearing steel 100Cr6 could be avoided for a temperature range from 800 to 900 C and a holding time of one hour by a combination of evacuate the furnace and using a certain nitrogen flow as protective gas. At lower temperatures small amounts of ferrite caused by an increased diffusion rate of carbon lead again to a surface decarburisation up to a depth of 2 {mu}m. It was proved that with an evacuation of the X-Ray beam path at constant power of the X-Ray source the intensity of ...
Fe{sub x}Zn{sub 1-x} alloys were electrochemically deposited on aluminum substrates from a sulfate bath. The K{beta}/K{alpha} x-ray intensity ratios of Zn and Fe in Fe{sub x}Zn{sub 1-x} thin films have been experimentally studied. The energy dispersive x-ray fluorescence (EDXRF) technique was used to measure K x-ray photons. Samples were excited by using 59.5 keV photons emitted by a 50 mCi {sup 241}Am radioactive source. The emitted K x-rays were detected by an Ultra-LEGe detector having a resolution of 150 eV at 5.9 keV. In addition, the effect of bath composition on the phase structure was investigated by x-raydiffraction (XRD) analysis. The composition of the thin films was analyzed by atomic absorption spectrometry analysis. Iron content was shown to strongly affect the structure of Zn-Fe alloys. It was found that ...
FexZn1-x alloys were electrochemically deposited on aluminum substrates from a sulfate bath. The K?/K? x-ray intensity ratios of Zn and Fe in FexZn1-x thin films have been experimentally studied. The energy dispersive x-ray fluorescence (EDXRF) technique was used to measure K x-ray photons. Samples were excited by using 59.5 keV photons emitted by a 50 mCi 241Am radioactive source. The emitted K x-rays were detected by an Ultra-LEGe detector having a resolution of 150 eV at 5.9 keV. In addition, the effect of bath composition on the phase structure was investigated by x-raydiffraction (XRD) analysis. The composition of the thin films was analyzed by atomic absorption spectrometry analysis. Iron content was shown to strongly affect the structure of Zn-Fe alloys. It was found that the K-shell x-ray ...
Bi-U mixed oxides were synthesized by two methods and characterized by X-raydiffraction and X-ray photoelectron spectroscopy. The samples were tested for the catalytic oxidation of carbon monoxide by oxygen. A stepwise redox mechanism consistent with the kinetic results is proposed. (orig.).
The effect of resonance, observed in X-ray waveguide layered structures in a characteristic way influences the scattering properties of the films. It is well known that the resonant region in the reflectivity shows a series of minima, usually very deep and extremely narrow. The positions and depths of the minima depend only on X-ray waveguide and quasi X-ray waveguide film structural properties, on the X-ray wavelength and on the incident beam divergence. In the present work we propose and discuss the application of the X-ray waveguide and quasi X-ray waveguide film structures as a tools to experimental evaluation of some quantities related to X-ray reflectometric and diffractometric measurements, like the beam divergence, wavelength, or angular distance. Examples of application of X-ray waveguide as an excellent tool ...
A cyclic hexapeptide, annomuricatin A (the molecular formula: C27H38N6O7), was isolated from the seeds of Annona muricata. The types and sequence of the amino acids were confirmed by X-raydiffractionanalysis. The stereochemistry of the title cyclopeptide was clarified by X-ray crystallographic study. The backbone contains two b-turns, one is type I b-turn and the other is type II, which are stabilized by two transannular 41 backbone hydrogen bonds between Ala and Phe. There are intermolecular hydrogen bonds between the cyclopeptide and the solvent molecules which maintained the steady spatial arrangement in crystal.
New phosphates with NaZr{sub 2}(PO{sub 4}){sub 3} structure of the B{sub 0.5}FeTa(PO{sub 4}){sub 3}-type (where B-Ca, Sr, Ba) are synthesized and characterized by X-raydiffractionanalysis and IR-spectroscopy. The heating behavior of the phosphates is studied using high-temperature X-ray crystallography in the range 15-625 deg. C. The unit-cell parameters, the coefficients of thermal expansion {alpha}{sub a}, {alpha}{sub c} and their thermal expansion anisotropy |{alpha}{sub c} - {alpha}{sub a}| of the phosphates under study are determined and the dependences of these characteristics on the nature of cations are established and analyzed.
An x-raydiffraction technique for determining thin-film thickness is presented which should prove to be a valuable alternative to the array of spectroscopies (Rutherford backscattering spectrometry, Auger electron spectroscopy, etc.) currently favored for these measurements. Some of the virtues of this x-raydiffraction approach are its nondestructive nature, fast data acquisition rate (enabling in situ observations), thickness resolution better than 5 nm, and conventional equipment requirements. Results are shown for Pd/sub 2/Si thin films grown during isothermal annealing of Pd coatings (100 nm) on Si at 200 /sup 0/C for various amounts of time. A comparison of these x-ray measurements with Rutherford backscattering spectrometry data taken from the same specimens is used to demonstrate the validity of the x-ray technique.
X-raydiffraction offers a unique combination of advantages for kinetic study which include the non-destructive nature of the measurement, the use of bulk crystals, and the convenience of the experimental arrangements. These attributes and the availability of position-sensitive detectors and high-flux synchrotron radiation sources make this technique most useful for in situ, dynamical investigations. When using diffraction techniques to determine a diffusion coefficient, the principle of analysis entails a scattering theory and a kinetic model. The former allows the kinetic parameter(s) to be extracted from measured intensity, while the latter relates the kinetic parameter(s) to the diffusion coefficient(s). Three examples are demonstrated: (1) Palladium Silicide (Pd{sub 2}Si) Layer Growth on Silicon, (2) Decomposition of an Ni-12.5at%Si Superalloy, and (3) Short-range Ordering in Cu-Au Solid Solutions.
The author's achievements in the title field are summarized and discussed. The following topics are dealt with: (i) principles of radionuclide X-ray fluorescence analysis; (ii) mathematical methods in X-ray fluorescence analysis; (iii) Ross differential filters; (iv) application of radionuclide X-ray fluorescence analysis in the coal industry (with emphasis on the determination of the ash content, sulfur content, and arsenic content of coal); and (v) evaluation of the X-ray fluorescence analyzer from the radiological safety point of view. (P.A.).
Single crystals of semi-organic L-histidine hydrobromide have been grown by slow evaporation technique from a mixture of L-histidine and hydrobromic acid in aqueous solution at ambient temperature. From high-resolution X-raydiffractionanalysis, the crystalline perfection of the grown crystal has been studied. Single crystal X-raydiffraction analyses, Nuclear Magnetic Resonance spectral analysis, Thermo-Gravimetry (TG), Differential Thermal Analysis (DTA) and hardness test have been employed to characterize the as-grown crystals. The UV cutoff wavelength of the grown crystal is below 300 nm and has a wide transparency window, which is suitable for second harmonic generation of laser in the blue region. Nonlinear optical characteristics have been studied using Q switched Nd:YAG laser (#lambda#=1064 nm). The second harmonic generation ...
The structural parameters of various Haegg phases (H or M_n_+_1AX_n phases) are studied experimentally by x-ray and electron spectroscopies, x-raydiffraction, and ab initio full potential as well as full mutiple scattering theoretical calculations. Experimentally it was found that the structure of all ternary compounds analyzed herein are relaxed. The values of the lattice parameters and relaxations obtained from ab initio calculations are in excellent agreement with those deduced from the analysis of the experimental data. The bonding scheme has been analyzed and the charge transfer between constituting atoms determined. It is demonstrated that the strength and electrical transport properties in these materials are principally governed by the metallic planes. For the solid solution (Ti_0_._5Nb_0_._5)_2AlC, the most salient result is that the basal planes are corrugated, which could explain the solid ...
The NiO-samaria doped ceria (SDC) composite powders were prepared by spray pyrolysis technique at temperatures between 400 and 1000 C. The variation of the particle structure was investigated by X-raydiffraction (XRD), X-ray absorption fine structure (XAFS), scanning electron microscope (SEM), and transmission electron microscope (TEM)-energy-dispersive X-ray spectroscopy (EDS). The thermal analysis of raw materials was also carried out. The following facts became clear in this study. Ceria and nickel have been already separated at 400 C. Samaria is amorphous phase below 600 C, and is dissolved in ceria at 600 C or higher. Samaria is distributed uniformly inside the particles before dissolving in ceria. The thermal decomposition temperatures of metal nitrate are: cerium < nickel < samarium. The results of these analyses were explained without contradiction. It was ...
Nitriding leads to improved tribological and corrosive properties of iron alloy components. In order to study the effect of plasma nitriding parameters on the structure of compound layer and diffusion zone, a systematic variation of process parameters, temperature and process gas atmosphere has been carried out. Metallographic inspection, X-raydiffraction and glow discharge optical spectroscopy analysis (GDOES) were used in this investigation. The results clarified that depending on the amount of nitrogen in the gas atmosphere nitrided layers with and without compound layer can be generated in the surface of M2 tool steel for temperatures from 350 C to 500 C. For plasma nitriding in 5 vol.% Nitrogen and 95 vol.% Hydrogen no compact compound layer was formed. The gas mixture of 76 vol.% Nitrogen resulted in compound layer formation for all temperatures from 350 C to 500 C. X-ray phase ...
Phase transformations occuring during cold deformation in hardened #alpha#+#beta# titanium alloy of the Ti-Al-Mo-Zr-Sn-Si system with 10% summary content of alloying elements are studied by X-raydiffractionanalysis. Two stages of trapsformation of metastable #alpha#''-phase are found. A conclusiop is made that ability of the alloy containing #alpha#''-phase to cold deformation is determined by the presence of favourable texture, by high degree of metastability and by volume portion of #alpha#''-phase in the alloy structure.
The nine papers presented at this conference cover the following topics: the systematization, condensed description, and prediction of sets of anion exchange extraction constants on the basis of their statistical computer treatment; characteristics and uses of solid extractants containing D2EHPA and TBP for separating the transplutonium elements; enrichment of americium 242m and americium 242 by the Szilard-Chalmers method; an x-raydiffraction pattern analysis for transplutonium compounds; the radiation chemistry of americium; and the effects of alpha irradiation on the behavior of americium in perchlorate solutions.
The influence of microalloying vanadium or titanium on improving the corrosion resistance of mild steel in saturated calcium hydroxide solution was investigated. Potential-time, potentiodynamic polarization, and impedance measurement techniques were employed. The corrosion products have been examined by infrared and X-raydiffractionanalysis and by scanning electron microscopy. It has been shown that the grain refining, due to microalloying, plays an important role in enhancing the corrosion resistance of steel. Scales of calcite and iron oxides on top of a protective oxide are formed on the investigated steels.
Glow discharge plasma nitriding of AISI 304 austenitic stainless steel has been carried out for different processing time under optimum discharge conditions established by spectroscopic analysis. The treated samples were analysed by X-raydiffraction (XRD) to explore the changes induced in the crystallographic structure. The XRD pattern confirmed the formation of an expanded austenite phase (#gamma#_N) owing to incorporation of nitrogen as an interstitial solid solution in the iron lattice. A Vickers microhardness tester was used to evaluate the surface hardness as a function of indentation depth (#mu#m). The results showed clear evidence of surface changes with substantial increase in surface hardness.
The results of a combined investigation of splat-quenched Fe-Csub(x) (x<0.05) alloys by resistivity, X-raydiffraction and Moessbauer spectroscopy are presented. The residual resistivity increases linearly with the carbon content (#DELTA#rho=5#mu##OMEGA#cm/at.%) with a slope identical to that observed in the dilute ferritic phase. X-raydiffraction reveals the presence of a martensite structure in addition to a small fraction of residual austenite; the dependence of the a and c lattice parameters on xsub(c) agrees with earlier measurements. A detailed investigation of the relative reflexion intensities shows that the as-quenched martensites consist of a mixing of massive martensite and tetragonal martensite for low carbon content and of tetragonal martensite only for xsub(c) approximately 0.05. The Moessbauer spectra reveal 3 or 4 magnetically non equivalent iron sites. From a detailed ...
Nano-sized zinc oxide was synthesized and deposited onto cellulosic fibers using the sol-gel process at ambient temperature. The prepared materials were characterized using several techniques including scanning electron microscopy, transmission electron microscopy, diffuse reflectance spectroscopy, X-raydiffraction and thermogravimetric analysis. X-raydiffraction studies of the ZnO-coated fiber indicate formation of the hexagonal crystal phase which was satisfactory crystallized on the fiber surface. The electron micrographs show formation of zinc oxide nanoparticles within 10-15 nm in size which have been homogeneously dispersed on the fiber surface. The prepared materials show significant photocatalytic self-cleaning activity, which was monitored by diffuse reflectance spectroscopy. The photoactivity was studied upon measuring the photodegradation of methylene blue and eosin ...
Coal demineralization mechanism and its optimum condition were studied by hydrothermal reaction between Ca(OH)2 and quartz as a coal demineralization model. In experiment, the mixture of powder quartz and Ca(OH)2 water slurry was subjected to reaction in an autoclave under spontaneous pressure at 175-340{degree}C. After dried in N2 gas atmosphere at 105{degree}C, the reaction product was analyzed by X-raydiffraction, thermo-balance and differential thermal analysis. In measurement of quartz conversion, the specimen was analyzed by X-raydiffraction after removal of bound water by heat treatment at 850{degree}C. The mixture of clean coal deashed by NaOH and a fixed amount of quartz was also used as specimen for experiment. As the experimental result, dicalcium silicate hydrate was mainly produced at 175{degree}C, and the product changed into xonotlite through tobermorite by longer ...
Discusses methods for determining ash content in coal using backscattering in X-ray fluorescence. The following aspects are evaluated: principle of ash content determination, energy sources, factors that influence measurement accuracy, reliability. Types of X-ray fluorescence analyzers developed in Czechoslovakia and manufactured in the Czech Republic are comparatively evaluated. Operation of the RPM 113.1 radionuclide X-ray fluorescence analyzer developed by the PAR company and used for measuring ash content in coal and coal calorific value is discussed. 7 refs.
The solid state reaction between a Pd thin film and a Si substrate produces a single new phase, Pd/sub 2/Si, for temperatures <700/sup 0/C. When the substrate is a single crystal of (111) surface orientation, this process is particularly interesting because the silicide grows epitaxially. Growth of epitaxial interfacial Pd/sub 2/Si was the focus of this study using X-raydiffraction techniques.
The design of the time-resolved x-raydiffraction experiments reported in this and an accompanying paper was based on direct measurements of enzyme phosphorylation using [gamma-32P]ATP that were employed...Full Text Available
A series of novel triazolinones were synthesized and their structures were characterized by 1H NMR, elemental analysis and single-crystal X-raydiffractionanalysis. The herbicidal activities were evaluated against Echinochloa crusgalli (L.) Beauv., Digitaria adscendens, Brassica napus and Amaranthus retroflexus. The herbicidal activity data indicated that the title compounds had higher activities with substituted benzyl group moieties than with other groups such as sulfonyl, alkyl, etc. To further investigate the structure-activity relationship, comparative molecular field analysis was performed on the basis of herbicidal activity data. Both the steric and electronic field distributions of comparative molecular field analysis are in good agreement in this work. The results showed that a b...
The determination of residual stress (RS) in case-hardened steel gear truck synchronisers coated with thermal sprayed molybdenum was carried out using neutron and synchrotron X-raydiffraction. Two samples with different coating thicknesses (about 120 ?m and 1.4 mm) and different steel substrates (16MnCr5 and SAE4140, respectively) were investigated. Microanalysis revealed substantial porosity in both samples and some debonding was observed between the thin coating and the substrate. The bulk hardness of the SAE 4140 proved to be much higher than the 16MnCr5 and the surface case-hardening increased it by a further 20%. The full three-dimensional stress depth-profile was determined by neutron diffraction (ND) in both the coatings and the substrates, while synchrotron radiation allowed a dep...
The physical foundations and methodology are described of radionuclide X-ray fluorescence analysis. The sources are listed of air, water and soil pollution, and the transfer of impurities into biological materials is described. A detailed description is presented of the sampling of air, soil and biological materials and their preparation for analysis. Greatest attention is devoted to radionuclide X-ray fluorescence analysis of the components of the environment. (ES).
Radionuclide X-ray fluorescence analysis was used for the determination of iron, calcium, potassium, copper, manganese and zinc in waste water from the production process of citric acid.
Radionuclide X-ray fluorescence analysis was used for the determination of iron, calcium, potassium, copper, manganese and zinc in waste water from the production process of citric acid. (author).
Certain applications are described of radionuclide X-ray fluorescence analysis in the ore dressing industry, in the manufacture of building materials, in metallurgy, pharmacy, in the chemical, photographic and paper industries, in space exploration, in archeology and for measuring the thicknesses of thin layers of coatings. (ES).
A method has been developed to optimize the energy resolution of a horizontally focusing monochromator. The method consists of determining the optimum radius of curvature of the cylindrically bent monochromator crystal by minimizing the total diffractedX-ray flux measured through an X-ray absorption foil. When measured at an absorption edge a global minimum can be identified, which corresponds to the minimum energy band accepted along the entire length of the crystal. Experimental verification of this method has been validated by comparing X-ray fluorescent scans taken for a series of crystal curvatures and by directly measuring the X-ray beam profiles at the corresponding points. The actual optical configuration and asymmetric-cut parameter of the focusing monochromator on beamline X4C at the National Synchrotron Light Source are modeled and ray tracing simulations of the optical ...
Determination of Mn, Fe, Ni, Cu, Zn, and Pb in human soft tissues by radionuclide X-ray fluorescence analysis (using "2"3"8Pu and "1"0"9Cd sources) is described. The results of multielement XRS analysis of selected human tissues are tabulated. They are in good agreement with the literature data. It is concluded that X-ray fluorescence technique is a suitable method for trace element determination. (author).
In the present paper the tribological behavior of the coatings are discussed. Duplex coatings were applied on cold working steel 100Cr6. Samples were plasma nitrided at different thickness of plasma surface layers. TiN was deposited with a classic BALZERS PVD equipment and subsequent ion implantation. Ion implantation was provided with N{sup 5+} ions. The other samples were produced with IBAD technology in DANFYSIK chamber. Wear resistance and exchanges of friction coefficient were measured with on-line test using special designed tribology equipment. Following the tests, the wear zone morphology and characteristics of surface layer structure as well as important properties were investigated by scanning electron microscopy (SEM) and X-raydiffractionanalysis (XRD). Scratch adhesion testing was performed using commercially available equipment. Energy dispersive X-rayanalysis (EDAX) ...
The finest particle size fractions ({le} 25 {mu}m) in four fly ash samples from fluidised bed combustion of three biomass based fuels and a municipal solid waste fuel were size separated using a centrifugal SPLITT fractionation cell. The ashes were separated into different size fractions and the cadmium concentration, partition and speciation in each separated fraction were then investigated in relation to their possible leaching. The fractionation was evaluated by environmental scanning electron microscopy, which also provided indications of the associations between Cd and other main elements on the particles through the use of X-ray fluorescence mapping. The total concentration of Cd in each fraction was determined by AAS analysis which showed different dependence on the ash particle size in the case of biomass or waste fuels. In addition, the speciation of Cd in each fraction, investigated by sequential chemical extractions and ...
The results of X-ray and neutron diffraction experiments on molten alkali halides in which some data of our experiments by X-raydiffraction such as those of molten LiCl, NaCl, KCl, LiBr and KBr are included were summarized. The first peak positions in the radial distribution function in molten alkali halides by X-ray or neutron diffraction experiments are always longer than those by computer simulations and the differences of 0.1 -- 0.3 A exceed the experimental error. It seems to be due to the deformation of the electron shell. In the computer simulation, the shell model which has the spherical deformation was expected to have a closer value of the first peak position to the experimental one than the rigid ion model by taking the polarization of ions. However, no change in the first peak position was found. Therefore, the non-spherical deformation of electron ...
The results of X-ray and neutron diffraction experiments on molten alkali halides in which some data of our experiments by X-raydiffraction such as those of molten LiCl, NaCl, KCl, LiBr and KBr are included were summarized. The first peak positions in the radial distribution function in molten alkali halides by X-ray or neutron diffraction experiments are always longer than those by computer simulations and the differences of 0.1 -- 0.3 A exceed the experimental error. It seems to be due to the deformation of the electron shell. In the computer simulation, the shell model which has the spherical deformation was expected to have more closer value of the first peak position to the experimental one than the rigid ion model by taking the polarization of ions. However, no change in the first peak position was found. Therefore, the non-spherical deformation of ...
A photon-induced x-ray fluorescence method allowing the simultaneous determination of iron, copper, zinc, bromine and rubidium in human blood and blood plasma samples is described. The method is reliable and has a good sensitivity for a wide range of elements. (author).
Applications of X-ray fluorescence analysis in coal mining and geology are briefly described based on results published in Czechoslovakia as well as abroad over the past 3 years. Particular attention is paid to the rapid determination of the ash content of coal using portable radionuclide X-ray fluorescence analyzers that are being developed in Czechoslovakia. (author).
A number of diagnostic X-ray units in Poland were subjected to analysis. The air kerma on X-ray tables was measured for the X-ray parameters used routinely during lumbo-sacral spine radiography of standard adult patient. Measurements of air kerma were performed using TLD made of lithium-fluoride. The doses received by patients in different X-ray departments can differ more than two orders of magnitude (from 0.42 mGy up to 72.11 mGy), for the same X-ray examination. The dose can be significantly reduced if fluorescent screens made from components of rare earth are used. (author). 10 refs, 1 fig., 2 tabs.
Nylon copolymer (PA6, 66) and ethylene propylene diene (EPDM) blends with and without compatibilizer were prepared by melt mixing using Brabender Plasticorder. The thermal stability of nylon copolymer (PA6, 66)/ethylene propylene diene rubber (EPDM) blends was studied using thermogravimetric analysis (TGA). The morphology of the blends was investigated using scanning electron microscopy (SEM). In this work, the effects of blend ratio and compatibilisation on thermal stability and crystallinity were investigated. The incorporation of EPDM rubber was found to improve the thermal stability of nylon copolymer. The kinetic parameters of the degradation process were also studied. A good correlation was observed between the thermal properties and phase morphology of the blends. By applying Coats ...
Beta-SiAlON powders have been synthesized using natural clay containing kaolin and quartz by carbothermal reduction and nitridation (CRN), then beta-SiAlON bonded corundum multiphase materials have been sintered using the as prepared powders. The results indicated that both the holding time and sintering temperature are relatively significant in accordance with optimal analysis by orthogonal method. Reaction process can be briefly interpreted by means of X-rayDiffraction and Difference Temperature Analysis as well as phase diagram principle. Bending strength and bulk density were measured in SiAlON in situ bonded corundum materials with doped various sintering agents. Furthermore, the relevant mechanical properties and microstructure were discussed in detail.
The microstructure evolution of nine samples from three Ir-base ternary systems, Ir-Nb-Hf, Ir-Nb-Ta, and Ir-Nb-Ti, was investigated by microstructure observation using scanning electron microscopy (SEM), composition map-analysis using electron probe microscopy analysis (EPMA), and phase determination using X-raydiffraction (XRD) patterns. The fcc/L1{sub 2} two-phase structure was detected in all the samples. Lattice misfits between fcc and L1{sub 2} phases were calculated. Ir-Nb-Ta and Ir-Nb-Ti alloys exhibited a microstructure quite similar to that of Ni-base superalloys, and the cuboidal L1{sub 2} precipitates in Ir-Nb-Ta and Ir-Nb-Ti alloys could maintain up to 1900 {sup o}C.
Interest in the tribological properties of plasma nitriding has increased substantially over the past years because plasma nitriding provides a high nitride depth and improved hard facing. The present study examines the tribological properties of AISI H11 plasma nitrided, hot-worked steel. Different nitriding temperatures and durations were considered. Characterization of the composite structures was investigated with wear tests, x-raydiffraction (XRD) analysis, scanning electron microscopy (SEM), and microhardness tests. The depth profile of the nitrided zone was measured using the nuclear reaction analysis (NRA) technique. Plasma nitriding affected the microhardness, wear properties, and morphology considerably. Increase in process temperature increased the nitride zone depth.
In this work AISI 1045 steel were duplex treated via plasma nitriding of chromized layer. Samples were pack chromized by using a powder mixture consisting of ferrochromium, ammonium chloride and alumina at 1273K for 5h. The samples were then plasma-nitrided for 5h at 803K and 823K, in a gas mixture of 75%N2+25%H2. The treated specimens were characterized by scanning electron microscopy (SEM), X-raydiffraction (XRD) analysis and Vickers micro-hardness test. The thickness of chromized layer before nitriding was about 8mm and it was increased after plasma nitriding. According to XRD analysis, the chromized layer was composed of chromium and iron carbides. Plasma nitriding of chromized layer resulted in the formation of chromium and iron nitrides and carbides. The hardness of the duplex layer...
X-raydiffraction, infrared spectroscopy, thermal analysis, scanning electron microscopy, and particle size analysis were used to characterize the product of the thiosulfate process. It was found to consist of a mixture of a solid solution of calcium sulfate in calcium sulfite hemihydrate, calcium sulfate dihydrate, and calcium carbonate. Reactions taking place on heating the byproduct were identified in oxidizing and reducing atmospheres. Pure calcium sulfite hemihydrate as well as solid solutions of CaSO[sub 4] in CaSO[sub 3] [center dot] (1/2)H[sub 2]O with different sulfate concentrations were synthesized in the laboratory. Thermal analyses of pure solid solutions proved that the higher the sulfate content, the higher is the dehydration temperature. Accordingly, taking SO[sub 4][sup 2[minus
Here in the present paper, we report on growth of stoichiometric and nonstoichiometric nanostructured heterojunction solar cell of CdS/CuInSXSe2-X varying X from 0 to 2 in the interval of 0.5 using cost effective, simple, chemical ion exchange method at room temperature on ITO glass substrate. The as-grown varying composition solar cells annealed at 200degreeC in air and characterized for structural, compositional, optical and illumination studies. The X-raydiffraction pattern obtained from CdS/CuInSXSe2-X solar cell confirms the formation of CuInSe2, CuInS0.5Se1.5, CuInS1Se1, CuInS1.5Se0.5 and CuInS2 phases having tetragonal structure with varying crystallite size from 19, 19.37, 28, 33 and 20nm respectively. The energy dispersive X-rayanalysis (EDAX) confirms the expected elemental com...
The efficiency of the synthesized zeolite NaY from rice husk ash (RHA) in the removal of Cr(III) from aqueous solution was studied. Zeolite NaY was synthesized from RHA via seeding technique and the identification of its structure was done by X-rayDiffraction (XRD) technique and the elemental analysis was carried out by X-ray Fluorescence (XRF). The physicochemical properties which were related to the use of the zeolite NaY as a sorbent was also investigated. The synthesized zeolite NaY has higher cation exchange capacity (CEC) than the commercial zeolite NaY due to the higher amount of sodium content in the synthesized as well as the lower ratio of silica to alumina. The synthesized zeolite NaY together with the commercial one as comparison was used in the sorption of the Cr(III) in aqueous solution by batch sorption experiments. The kinetic study showed that the Cr(III) uptake by both zeolites were ...
Homogeneous mixtures of Ce0.8Gd0.2O1.9 (GDC) and La0.6Sr0.4Co0.2Fe0.8O3 (LSCF) nanopowders were successfully synthesized using induction plasma by axial injection of a solution. The resulting nanocomposite powders consisted of two kinds of nanopowders with different mass ratio of GDC/LSCF, such as 3/7 and 6/4. The morphological features, crystallinity, and the phases of the synthesized powders were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), local energy-dispersive x-ray spectroscopy (EDS) analysis, and x-raydiffraction (XRD). The nanopowders are almost globular in shape with a diameter smaller than 100?nm and their BET specific areas are around 20?m2?g?1. The GDC and LSCF phases are well distributed in the nanopowders. In addition, suspens...
Iron oxide thin films have been obtained by spray pyrolysis using 100% methanolic and ethanolic solutions of iron tri-chloride. The films were deposited onto ITO-coated glass substrates. The preparative conditions have been optimized to obtain compact, pin-hole-free and smooth thin films which are adherent to the substrate. The structural, morphological and compositional characterizations have been carried out by X-raydiffraction, scanning electron microscopy and energy dispersive X-rayanalysis. The films deposited using ethanolic solution results into pure hematite; #alpha#-Fe_2O_3 thin films, however, films deposited using methanolic solution consists of hematite and maghemite-c phases of iron oxide. The films are nanocrystalline with particle size of 30-40 nm. The optical absorbance of the film was of the order of 10"5 cm"-"1. The optical band gap of films was found to be 2.26 and 2.20 eV for the ...
The next generation of synchrotrons and free electron laser facilities requires x-ray optical systems with extremely high performance, generally of diffraction limited quality. Fabrication and use of such optics requires adequate, highly accurate metrology and dedicated instrumentation. Previously, we suggested ways to improve the performance of the Long Trace Profiler (LTP), a slope measuring instrument widely used to characterize x-ray optics at long spatial wavelengths. The main way is use of a CCD detector and corresponding technique for calibration of photo-response non-uniformity [J. L. Kirschman, et al., Proceedings of SPIE 6704, 67040J (2007)]. The present work focuses on the performance and characteristics of the upgraded LTP-II at the ALS Optical Metrology Laboratory. This includes a review of the overall aspects of the design, control system, the movement and measurement regimes for the stage, and ...
Full text: The production of #beta#-sialon from kaolinite and carbon has been studied using Hulu Langat Kaolin and activated carbon as raw materials. The sintered temperature is shown to play a prominent role in the process of sialon conversion. Apart from temperature, nitrogen flow rate is also affect the production of #beta#--sialon. This study was carried out on the effect of additive, Y_2O_3 and Al_2O_3 at different temperature that will be mixed and sintered. The additives are expected to affect the formation of #beta#--sialon and Y-sialon upon the synthesis. The mineral and phase development was analysed using X-RayDiffraction technique (Rigaku Geigerflex) while its chemical compositions through X-Ray Fluorescent Spectrophotometer (Shimadzu XRF 1700) and the particle size distribution analysis through Particle Size Analyser (Horiba, CAPA 700). The observed changes in the microstructure were ...
A magnetic core/shell Fe3O4/FeMnOx catalyst was prepared by a simple oxidation-precipitation method. The catalyst was characterized by X-raydiffraction, transmission electron microscope, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis and cyclic voltammetry. The characterization studies verified that Fe3O4 core was coated with a layer of Fe-Mn oxide. The Fe3O4/FeMnOx was found to be an effective and stable heterogeneous catalyst for the discoloration of methylene blue (MB) in aqueous solution by H2O2. The high catalytic activity is due to the FeMnOx shell, which not only increased the surface hydroxyl groups, but also enhanced the interfacial electron transfer. The discoloration of MB could be due to the decomposition of H2O2 into ?OH ...
The resolution of X-raydiffraction microscopy is limited by the maximum dose that can be delivered prior to sample damage. In the proposed Serial Crystallography method, the damage problem is addressed by distributing the total dose over many identical hydrated macromolecules running continuously in a single-file train across a continuous X-ray beam, and resolution is then limited only by the available molecular and X-ray fluxes and molecular alignment. Orientation of the diffracting molecules is achieved by laser alignment. We evaluate the incident X-ray fluence (energy/area) required to obtain a given resolution from (1) an analytical model, giving the count rate at the maximum scattering angle for a model protein, (2) explicit simulation of diffraction patterns for a GroEL-GroES protein complex, and (3) the frequency cut off of the ...
The optoelectronic compounds of GaAs and ZnSe are difficult to analyze by PIXE (particle-induced X-ray emission) due to the strong absorption of the As and Se K{sub {alpha}} X-rays. As part of a program to investigate optoelectronic materials using ion beam techniques, we have explored the possibility of using the high sensitivity of PIXE to check these materials for stoichiometry and dopant concentrations. The K{sub {alpha}} X-ray intensity ratios of Ga to As and Zn to Se have been investigated using H beams of 0.5 to 2.5 MeV and He beams of 1.0 to 2.5 MeV. The variation in the X-ray intensity ratio with beam energy and target thickness is modelled in terms of the cross section for X-ray production and the absorption coefficients of the X-rays in the target. The results of this model show the experimental conditions that must be satisfied in order that the ...
The optoelectronic compounds of GaAs and ZnSe are difficult to analyze by PIXE (particle-induced X-ray emission) due to the strong absorption of the As and Se K_#alpha# X-rays. As part of a program to investigate optoelectronic materials using ion beam techniques, we have explored the possibility of using the high sensitivity of PIXE to check these materials for stoichiometry and dopant concentrations. The K_#alpha# X-ray intensity ratios of Ga to As and Zn to Se have been investigated using H beams of 0.5 to 2.5 MeV and He beams of 1.0 to 2.5 MeV. The variation in the X-ray intensity ratio with beam energy and target thickness is modelled in terms of the cross section for X-ray production and the absorption coefficients of the X-rays in the target. The results of this model show the experimental conditions that must be satisfied in order that the ...
Much research has been done to estimate the residual stress on a dissimilar metal weld. There are many methods to estimate the weld residual stress and FEM (Finite Element Method) is generally used due to the advantage of the parametric study. And the X-ray method and a Hole Drilling technique for an experimental method are also usually used. The aim of this paper is to develop the appropriate FEM model to estimate the residual stresses of the dissimilar overlay weld pipe. For this, firstly, the specimen of the dissimilar overlay weld pipe was manufactured. The SA 508 Gr3 nozzle, the SA 182 safe end and SA376 pipe were welded by the Alloy 182. And the overlay weld by the Alloy 52M was performed. The residual stress of this specimen was measured by using the Neutron Diffraction device in the HANARO (High-flux Advanced Neutron Application ReactOr) research reactor, KAERI (Korea Atomic Energy Research Institute). Secondly, FEM Model on the ...
Airborne lead particulates collected on a membrane filter were determined by the nondestructive X-ray fluorescence method. The gamma/X radionuclide source "2"4"1Am/Ag and a scintillation detector with a NaI/Tl crystal were used for the excitation and detection, respectively, of L X-rays of Pb. One can say, with reference to the obtained results, that the sensitivity and accuracy of the measurement is more than adequate for monitoring the Pb level in air. (author).
The basic principles of determination of the ash content of coal by the title methods are outlined. A brief technical characteristic of the ash meters and radionuclide X-ray fluorescence analyzers manufactured by the PAR company is presented. (Z.S.). 4 figs., 7 refs.
Smith-Purcell (S-P) radiation is produced when electrons graze the surface of a grating. Calculations based on the theory of diffraction radiation show that, given severe restrictions on e"--beam quality, S-P radiation is highly efficient. Efficient S-P x-ray generation requires relativistic e"- beams having a transverse momentum and dimension whose product approaches the Heisenberg uncertainty limit.
The possible existence of preferential B-site disorder in A-15 compounds recently claimed on the basis of x-ray powder diffraction data but questioned from the viewpoint of known phase diagrams is examined for some Nb-based compounds of this type. It is concluded that x-ray powder data do not allow the determination of both order and compositional variables as suggested, and the latter must therefore be determined by some other method. (author).
Understanding the mechanical properties of biomedical devices is critical in predicting and preventing their failure in the body. Such knowledge is essential, for example, in the design of biomedical stents, which must undergo repeated strain over their ten year lifetimes without breaking. Computational models are used to predict mechanical response of a device, but these models are not complete; there are significant deviations from the predictions, especially when devices are subjected to repeated multi-axial loads. Improving these models requires comparisons with actual measurements of strained nitinol. Local measurements of the full strain tensor can be made using X-raydiffraction techniques, but they are currently limited to materials whose grain size is larger than the X-ray beam size or require several diffraction patterns produced by rotation of the sample. Nitinol stents are nanocrystalline, ...
We have investigated the microstructure evolutions in the Ti17 near #beta# titanium alloy during heat treatments. The phase transformation has first been studied experimentally by combining X-raydiffractionanalysis, electrical resistivity and microscopy observations. From a series of isothermal treatments, a IT diagram has been determined, which takes into account the different morphologies. Then, a Johnson-Mehl-Avrami-Kolmogorov (JMAK) model has been successfully used to describe the phase transformation kinetics during either isothermal or cooling treatments. Finally, the coupling of the JMAK model to the finite element software ZeBuLoN allowed us to investigate the evolution of the spatial distribution of the different morphologies during the cooling of an aircraft engine shaft disk after forging.
Reduction of silver myristate (AgMy) under mild thermal reaction conditions in a dipolar aprotic solvent i.e. N, N-dimethylformamide (DMF) has been carried out. UV-visible absorption measurements of dried and re-dispersible brown flocculants showed broad features of surface plasmon resonance (SPR) due to silver nanoparticles. The freshly isolated particles showed absorption bands at 414 and 485 nm, respectively, due to inter-particle coupling or clustering of silver ions and silver atoms. X-raydiffraction (XRD) pattern of fcc zero-valent silver resulted in crystallite size of about 10 nm. Scanning electron microscopy (SEM) revealed formation of rod shaped silver with increasing reaction temperature. Thermal analysis (TGA) showed about 10% weight loss due to organic capping.
To study the effect of CuO on the electrochemical properties of MgNi alloy, the MgNi-xCuO (x = 3, 5 and 10 wt%) composites were prepared by ball-milling method. The X-raydiffraction (XRD) analysis showed that the structures of the composites were amorphous. The cycle stability of the composites was improved compared to pure MgNi alloy due to the enhancement of the anti-corrosion property in the alkaline electrolyte, and the composite with 5 wt% CuO ball-milled for 15 h exhibited the best performance. Electrochemical impedance spectroscopy (EIS) and potential-step measurements indicated that the electrochemical kinetics of the composites was improved.
Phase and structural transformations in a multicomponent (5.05 mas.% Mo-4.95V-3.00Cr-3.05Al) metastable #beta#-titanium alloy on aging after plastic deformation are studied using methods of electron microscopy and X-raydiffractionanalysis. The alloy is deformed by twinning in a #left brace#332#right brace# system, and even at initial stages the formation of a twin skeleton takes place in the structure, on further loading the deformation of the skeleton is by secondary twinning resulting in a high plasticity of the alloy. On annealing mechanical twins transform into #alpha#-phase - a ductile twin skeleton is replaced by a rigid skeleton of #alpha#-phase plates. The aging enhances the yield strength of the alloy but decreases sharply its plasticity
Three new phases with compositions, LaSr_2FeTiO_7, NdSr_2FeTiO_7 and GdSr_2FeTiO_7, were prepared by the traditional ceramic method. Lazy-Pulverix analysis of the X-raydiffraction data suggests that the phases crystallize in the RP-type (n = 2) structure in the space group, I4/mmm. The cell dimensions along the c-axis decrease with decrease in size of the rare earth ions. Electrical resistivity, as a function of temperature, shows that the materials are insulators and the resistivity decreases with decrease in the size of the rare earth ion, which is attributed to increase in the three-dimensional character. (author)
Nanocrystalline chromium oxynitride films were deposited by reactive RF magnetron sputtering of metallic chromium target in argon and helium atmospheres. The paper deals with consequence of increase in oxygen partial pressure on structural, hydrophobic and optical properties of chromium oxynitride films. The film stoichiometry changes from CrN and Cr2O3 to only Cr2O3 with increase in oxygen partial pressure as evident from X-RayDiffractionanalysis in both cases. The average crystallite size decreases with increase in oxygen partial pressure for both gas atmospheres. The thickness calculated from transmission data and surface profilometer are in good harmony with each other. The deposited films are hydrophobic by nature and the contact angle of the films varies as a function of surface ro...
Modeling calculations on the solubility of americium have indicated that basic americium carbonate, and not americium trihydroxide, is the solubility-controlling solid in the pH range from 6 to 10 under the influence of atmospheric CO{sub 2}. The solubility of crystalline {sup 243}AmOHCO{sup 3} has been investigated in batch experiments in near-neutral and basic solutions as a function of dissolution time in 0.1 M NaClO{sup 4} at room temperature under oxic conditions. After the solutions reached steady-state conditions, the influence of dissolved solids on the americium concentration in the supernatant solution was studied by utilizing several experimental methods to separate the solution phase from the solid. The solids were characterized by X-ray powder diffractionanalysis.
Indium sulfide thin films consisting of porous network of nanoplatelets, have been deposited using chemical bath deposition (CBD) method onto the tin-doped indium oxide (ITO) coated glass substrate. Aqueous solutions of indium sulfate and thioacetamide have been used as indium and sulfur precursors. As a complexing agent, acetic acid was used. The chemically deposited indium sulfide thin films were examined for their structural, surface morphological and optical characterizations. The X-raydiffractionanalysis revealed the formation of the cubic b-In2S3 onto the substrate. From scanning electron micrograph, it is observed that the surface of substrate is covered by nanoporous platelets type morphology. The optical studies showed a direct band gap of 2.84eV for indium sulfide platelets. Ph...
The phase composition and microstructure of O'-sialon prepared from Chinese coal gangue have been studied. The use of Si powder is more effective than that of activated carbon or mainly carbon with a little silicon for reduction-nitridation. For specimens with 40% Si addition, more than 80% of O'-sialon may be obtained when nitrided at 1500 degree sign C. The formed O'-sialon was characterized by X-raydiffraction (XRD) and scanning electron microscope (SEM). The parameters for O'-Sialon preparation are optimized by computer pattern recognition program based on principal component analysis, the target parameter optimum regions with higher relative content of O'-Sialon was indicated by this way.
The present study is focused on preparation of nano composite materials and the effect of citric acid on their different properties. The formation of nano HA and its interaction with chitosan (C), gelatin (G) polymers and citric acid (CA) materials were studied. The Fourier Transformed Infrared Spectroscopy (FT-IR), X-raydiffraction (XRD), thermo-gravimetric analysis (TGA), transmission electron microscope (TEM), and scanning electron microscope (SEM) were used to characterize these composite materials. The compressive strength (CS) was also measured to know the reinforcement of the prepared composites. The results show that carboxylic and amino groups play crucial role for HA formation on chitosan-gelatin polymeric matrix in the presence of citric acid (CA). The formation of nano HA part...
The present investigation deals with the synthesis of nanostructured nickel ferrite (NiFe2O4) and their liquid petroleum gas-sensing characteristics. The 15-20nm size nickel ferrite has been synthesized at 700degreeC by a simple molten-salt route using sodium chloride as grain growth inhibitor. These nanoparticles exhibit significantly high response towards liquid petroleum gas (LPG) in comparison with ethanol vapor, hydrogen sulfide, ammonia and hydrogen. The gas response towards various gases at their 200ppm concentrations is investigated at 200-450degreeC. Different characterization techniques have been employed, such as differential thermal analysis, X-raydiffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high resolution transmission elec...
Commercially available organoclay (Closite 30B) was modified by using 3-aminopropyltriethoxysilane (APS) via a silylation reaction. Sodium clay (Closite Na) was treated by APS directly as a control. Such modified clays were further melt-compounded with polybutylene terephthalate (PBT). The morphology and properties of the modified organoclays were characterized with X-raydiffraction (XRD), transmission electrical microscopy (TEM), Infra-red spectroscopy, contact angle measurement, and thermogravimetric analysis (TGA). The effects of modified clays on the crystallization behavior of PBT were characterized by differential scanning calorimetry. The basal spacing of Closite Na was enlarged from 1.01 to 1.41 nm after APS treatment, indicating that the APS was intercalated into the clay interga...
Sintered glass-ceramics have been produced using municipal incinerator solid residues and glass cullet or an inert waste, from feldspars processing, as sintering aids. The capability of three different mixtures, either previously vitrified or not, to be sintered was investigated by means of linear shrinkage, water absorption and bulk density measurements, and by X-raydiffractionanalysis and scanning electron microscopy observations. Particular attention has been addressed to the study of particle size effect on the sintering process. The conclusions that can be drawn from the experimental study are that the preliminary vitrification step is essential in order to obtain a dense sintered glass-ceramic product in the 850-1050 C temperature range developing silicate crystalline phases. The optimal powder particle size that confers a good densification degree was found to be < 45 {mu}m. (orig.)
The total hemispherical emittance of an oxide film that formed on 6061-T6 aluminium alloy parts in the Tower Shielding Reactor-II at Oak Ridge National Laboratory was measured from 295 to 773 K using an emissometer and/or a calorimeter. The emittance of this film was critically needed for heat transfer calculations in a simulated loss-of-coolant accident of the reactor. X-raydiffractionanalysis identified the film as boehmite (Al_2O_3 x H_2O), which dehydrated to alumina (Al_2O_3) upon heating above 473 K. The measured emittances for the alumina film are in excellent agreement with published values for anodized aluminum films and for bulk alumina. Published values of the emittance of boehmite could not be found for comparison, but evidence is presented that some anodization processes for aluminum yield boehmite and not alumina films.
The effect of the composition of multicomponent Zr-Ti-V-Mn-Cr-Ni alloys on their hydrogen-storage capacity and on the rate of electrosorption/desorption hydrogen was investigated under potentiodynamics as well as single-pulse and long-term galvanostatic conditions. The main characteristics of alloys and alloy electrodes were determined by their structural analysis by means of X-raydiffraction and scanning electron microscope, by specific surface area test and by determination of the hydrogen absorption/desorption isotherms in the gas/solid phase system. It was found that only the alloys with a manganese content below a threshold could be used as electrode materials for Ni-MH batteries, whereas the modification of the electrode material by micro-encapsulation of alloy particles should limit the dissolution of manganese from the electrode material in a strong alkaline solution. (orig.)
We have investigated the effect of manganese (Mn) doping on properties of nanosized biphasic calcium phosphate powders and their dense bodies. Manganese levels of 0.6, 1.3, 1.9, 4.3, 7.0 and 11.9at.% were successfully incorporated into biphasic calcium phosphate via a sol-gel route. The prepared powders were calcined at temperatures of 500-1200^oC. The X-raydiffractionanalysis revealed that a mix phase comprising of hydroxyapatite and @b-tricalcium phosphate were present, however the content of each phases in the structure was affected by the Mn content. The studies found that the largest portion of @b-tricalcium phosphate was detected at 4.3at.% Mn doping. The incorporation of Mn has also greatly increased the crystallinity of the biphasic calcium phosphate powder due to progressive den...
In this project, nanocrystalline SnO2 powders were successfully prepared by (a) citrate sol-gel and (b) direct precipitation methods. Powders were characterized using thermal analysis techniques (DTA-TG-DSC), X-ray powder Diffraction (XRD), surface area (BET) and electrical conductivity measurements. XRD patterns showed the presence of the cassiterite structure. SnO2 particles, prepared through sol-gel method exhibit crystallite sizes in the range from 3.1 to 22.3 nm when the gel is heat treated at different temperatures up to 900?C. SnO2 nanocrystallites prepared by the precipitation method are comparatively larger in size. The higher specific surface area was obtained for the powder prepared using sol-gel method and the obtained average grain size (d) is relatively large compared with th...
Some results and experimental procedures of laboratory are reported in the frame of researches conducted for the development of new nanostructured composite materials. These new materials, which are constituted by an organic phase: the polymer and an inorganic phase: the silicate, are being strongly investigated nowadays so it is expected that they could provide, among other, better electrical insulation properties and flame-delay in electrical and electronic applications. The laboratory experimental work has been developed from two families of polymers, thermoplastics and thermosets and clays silicates providing lamellar type. There are now some preliminary results, such as obtaining thin films of these nanocomposite materials, their complete characterization by X-raydiffraction, scanning microscopy and thermogravimetric analysis, they do well to wait for future research activities. (author)
Bio-inspired palladium nanoparticles were synthesized by using banana peel extract (BPE), a non-toxic eco-friendly material. Boiled, crushed, acetone precipitated, air-dried peel powder was used to reduce palladium chloride. The palladium nanoparticles were characterized by using UV-Visible spectroscopy, scanning electron microscope-energy dispersive spectra (SEM-EDS) and X-raydiffraction (XRD) analysis. Dynamic light scattering (DLS) studies revealed the average size of nanoparticles to be 50nm. Fourier transform infra red spectroscopy (FTIR) implicated the role of carboxyl, amine and hydroxyl groups in the synthetic process. This paper thus describes a novel green method for the synthesis of palladium nanoparticles.
The principle is described of X-ray fluorescence analysis and the manner of detecting the emitted characteristic radiation. The advantages are presented of radionuclide X-ray fluorescence analysis which consist primarily in the possibility of conducting a totally non-destructive analysis, and of accurate and relatively narrow localization of the analyzed area, the simultaneous qualitative and quantitative determinations of a large number of elements in the order of concentrations 10"1 to 10"-"4%, stability of excitation radiation flux, simple design and relatively low capital costs. The so-called matrix effect is pointed to. A number of examples is given of the use of the cited method, including its use in the analysis of art objects. (J.B.).
A high degree of structural perfection is an essential requirement for CdTe crystals used as substrates for the epitaxial growth of CdHgTe alloys. Here, a method for the evaluation of the structural perfection of CdTe crystals is proposed which is based on X-raydiffraction measurements using both two-crystal and three-crystal diffractometers (differential version). The method makes it possible to obtain more information on structural perfection both at the crystal surface and within the crystal body.
Hydroxyapatite samples were produced by two different wet-chemical methods, and characterized by x-raydiffraction, infrared and compression strength measurements. The x-raydiffraction measurements were simulated using the Rietveld method, and structural data as lattice parameters and average crystallite size were obtained. The infrared spectra showed the presence of CO$_3^{2-}$ ions in all samples, indicating a contamination by these ions. By mixing samples produced by both methods, a bioceramic was obtained and, after sintering, samples with very high compression strengths (26--30 MPa) were obtained.
The transformation of Pd/Si to Pd{sub 2}Si/Si is investigated using depth-resolved positron annihilation, x-raydiffraction and Auger electron spectroscopy studies. The observed defect-sensitive positron S-parameter value of 1.022-1.054 indicates the existence of divacancies across the silicide/silicon interface and Si substrate region. Our experimental observation of vacancy defects is consistent with the model proposed for excess vacancy generation across the interface consequent to Si diffusion. (letter to the editor)
X-raydiffraction enhanced imaging (DEI) is one of X-ray phase-contrast imaging methods, which is applied to inspect internal structures of weakly absorbing low-Z samples. The key problem of the DEI is how to extract phase information which is expressed by refraction-angle images from a series of DEI images measured in different positions of the rocking curve of the analyzer. Three effective extraction methods are presented in this paper: the statistical geometric-optics-approximation method, the maximum refraction-angle method and the Gaussian curve fitting method. They are compared with the existing methods, such as the D. Chapman's geometric optics approximation method and the multiple-images statistical method. A 2D computer simulation experiment is performed to draw comparisons of these methods. The experimental results prove that the above three methods have more precision of refraction-angle values than ...
X-raydiffraction enhanced imaging (DEI) is one of X-ray phase-contrast imaging methods, which is applied to inspect internal structures of weakly absorbing low-Z samples. The key problem of the DEI is how to extract phase information which is expressed by refraction-angle images from a series of DEI images measured in different positions of the rocking curve of the analyzer. Three effective extraction methods are presented in this paper: the statistical geometric-optics-approximation method, the maximum refraction-angle method and the Gaussian curve fitting method. They are compared with the existing methods, such as the D. Chapman's geometric optics approximation method and the multiple-images statistical method. A 2D computer simulation experiment is performed to draw comparisons of these methods. The experimental results prove that the above three methods have more precision of refraction-angle values than existing ...
Crystalline ?-Al2O3 nanowires with diameter, 20?40?nm, length above 600?nm and aspect ratio above 30 have been successfully synthesized by thermal decomposition of boehmite (?-AlOOH) precursors obtained via hydrothermal route by using AlCl3, NaOH and NH3 as starting materials. Thermogravimetric analysis (TG), differential thermal analysis (DTA), X-raydiffraction (XRD), transmission electron microscope (TEM), selected area electron diffraction (SAED) and high resolution transmission electron microscope (HRTEM) were used to characterize the features of the as-made ?-Al2O3 nanowires and their ?-AlOOH precursors. The pH value of the solution and the mixed precipitant play important roles in the formation of ?-AlOOH nanowires. After calcination at 500?C for 2?h, the orthorhombic ?-AlOOH transf...
Eu-#alpha#-SiAlON (Eu_m_/_2Si_1_2_-_m_-_nAl_m_+_nO_nN_1_6_-_n) was synthesized with nominal compositions having small m and n values, by firing the powder mixture of Eu_2Si_5N_8, #alpha#-Si_3N_4, AlN, and Al_2O_3 at 1900 "oC for 6 h under 1 MPa nitrogen atmosphere. The ratio of the oxidation state of Eu"2"+/Eu"3"+ was estimated from the X-ray absorption fine structure (XAFS) measurement. The observed X-ray absorption near edge spectrum (XANES) showed that the Eu ion in Eu-#alpha#-SiAlON was mainly in divalent state but also coexisted with a small amount of Eu in the trivalent state. The crystal structure of Eu-#alpha#-SiAlON was refined by the Rietveld analysis of the X-ray powder diffraction patterns. The lattice constants of the samples increased with increasing m and n values. The excitation band of Eu-#alpha#-SiAlON ranged from the ultraviolet to the visible light region and a ...
The physical foundations are described of radionuclide X-ray fluorescence analysis (RXFA) and the table shows the values of K- and L-absorption thresholds and the K- and L-line energies of elements. The calculation of the intensity of characteristic radiation during RXFA proceeds from relations derived for conventional X-ray fluorescence analysis. The choice of the radionuclide source is ruled by the nature of the analysed substance and the used detection technique. The diagram shows the areas of radionuclide sources and the energy of the fluorescence radiation of elements. The table shows the spectra of radionuclide sources suitable for the purposes of RXFA measured by semiconductor Si(Li) and Ge(Li) detectors. (ES).
Recent X-ray and radio observations have identified a transient low-mass X-ray binary (LMXB) located only 0.1 pc in projection from the Galactic center, CXOGC J174540.0-290031. In this paper, we report the detailed analysis of X-ray and infrared observations of the transient and its surroundings. Chandra bservations detect the source at a flux of F_X = 2e-12 erg cm^-2 s^-1 (2-8 keV). After accounting for absorption both in the interstellar medium and in material local to the source, the implied luminosity of the source is only L_X = 4e34 erg/s (2-8 keV; D=8 kpc). However, the diffuse X-ray emission near the source also brightened by a factor of 2. The enhanced diffuse X-ray emission lies on top of a known ridge of dust and ionized gas that is visible infrared images. We interpret the X-ray emission as scattered flux from the outburst, and ...
The new nonlinear optical crystal Rb3V5O14 has been synthesized by solid state reaction and characterized by single-crystal X-raydiffraction, IR and thermogravimetric analysis. The crystal Rb3V5O14 crystallizes in the trigonal system with space P31m (No. 157), a=b=8.7134(12) A, c=5.2807(11) A and ?=90o, ?=90o, ?=120o, Z=1, ?=3.516 g/cm3. It is a layered structure that is very flat and strongly parallel to c. The V5O14 layer structure consists of corner-linked square and triangular pyramids. The layers are separated by Rb+ ions, which fit equally well on the V5O14 layer. The Kurtz powder SHG measurement, using 1064 nm radiation, showed that the second-harmonic generation efficiency of Rb3V5O14 is about two times that of KDP. -- Graphical abstract: The new nonlinear optical crystal Rb3V5O14 has been synthesized by solid state reaction and characterized by single-crystal X-ray ...
The x-raydiffraction technique described previously for measurement of growth kinetics of Pd/sub 2/Si layers from their solid state reaction couples has been extended by the use of a one-dimensional position-sensitive detector (PSD). Additionally, the method has been extended to include measurement of the Pd layer. A detailed description of the experimental arrangement and analytical procedures is presented. The kinetics of epitaxial Pd/sub 2/Si film growth were measured in situ over a range of 170--230 /sup 0/C. The PSD results, using data obtained from both the Pd/sub 2/Si and Pd layers, were able to confirm parabolic growth behavior for the Pd/sub 2/Si film. The rate constants followed Arrhenius behavior and yielded an activation energy of E = 1.32 +- 0.07 eV with a prefactor k/sub 0/ = 0.49 cm/sup 2//s for the Pd/sub 2/Si layer analysis and E = 1.34 +- 0.17 eV with a prefactor of 0.72 cm/sup 2//s for the Pd layer ...
by the radionuclide X-ray fluorescence analysis into several groups according to the atomic number of the determined element. Table I documents this. ...
Jan 22, 2011 ... dc.description.abstract, The progress in the development of a surface analysis tool based on the excitation of characteristic luminescence ...
Radionuclide X-ray fluorescence analysis was used for the determination of Cu, Y and Ba in very thin high-temperature superconducting films. The precision of the method is better than 3% for about 1 #mu#m thick films. The atomic emission ICP spectrometry was used to testify results of XRF analysis. An acceptable agreement of both methods was obtained. (author) 4 refs.; 2 tabs.
The {ital L}{sub 2}-{ital L}{sub 3} Coster-Kronig transition probability ({ital f}{sub 23}) in Tm was measured by multiparameter {ital K} versus {ital L} x-ray coincidence techniques. The Tm xrays were obtained from a radioactive source of {sup 169}Yb and were detected with cooled germanium and silicon detectors of high-energy resolution. Corrections were applied for the contribution of {ital K}{alpha}{sub 1} xrays to the {ital K}{alpha}{sub 2} x-ray peak and for the contribution of unresolved {ital L}{eta} xrays to the {ital L}{alpha}{sub 1,2} x-ray peak. The contribution of {ital K}{alpha}{sub 1} xrays to the {ital K}{alpha}{sub 2} x-ray peak was determined solely from the results of the coincidence measurements using a method of ...
The {ital L}{sub 2}-{ital L}{sub 3} Coster-Kronig transition probability ({ital f}{sub 23}) in Tm was measured by multiparameter {ital K} versus {ital L} x-ray coincidence techniques. The Tm xrays were obtained from a radioactive source of {sup 169}Yb and were detected with cooled germanium and silicon detectors of high-energy resolution. Corrections were applied for the contribution of {ital K}{alpha}{sub 1} xrays to the {ital K}{alpha}{sub 2} x-ray peak and for the contribution of unresolved {ital L}{eta} xrays to the {ital L}{alpha}{sub 1,2} x-ray peak. The contribution of {ital K}{alpha}{sub 1} xrays to the {ital K}{alpha}{sub 2} x-ray peak was determined solely from the results of the coincidence measurements using a method of ...
In this study nanocrystalline powders of yttria-stabilized zirconia (ZrO_2-8Y_2O_3) have been synthesized through 'polymerized complex method'. Zirconium chloride, yttrium nitrate, citric acid and ethylene glycol were polymerized at 80 "oC to produce a gel-like mass in which metallic ions were uniformly distributed. During the thermal treatment of dried gel, nanocrystalline powder was formed at 450 "oC and 650 "oC for 2 h. Thermal reactions and crystalline phase formation of the dried gel were investigated through thermal analysis and X-raydiffractionanalysis, respectively. The results of thermal analysis and XRD showed the formation of nanocrystalline powder at less than 600 "oC. Chemical bonding of the dried gel was investigated by Fourier transform infrared spectroscopy analysis. Morphology of powder calcined at 650 "oC was analyzed by scanning electron ...
The radionuclide X-ray fluorescence and particle induced X-ray emission methods were used for rapid and nondestructive analysis of metallic glasses. The methods were compared for accuracy and precision with the atomic absorption method. Some results of the analyses of Fe_xNi_8_0_-_xB_2_0 materials are briefly reviewed. The distribution of elements along the width as well as the length and a qualitative analysis of the composition of material surfaces are considered. (author).
Radionuclide X-ray fluorescence and particle induced X-ray emission methods were used for a rapid and nondestructive analysis of metallic glasses. The methods are compared in accuracy and precision with the atomic absorption method. Some results of analyses of Fe_xNi_8_0_-_xB_2_0 materials are briefly reviewed. The distribution of elements along the width and length, and a qualitative analysis of the composition of material surfaces are considered. (author) 3 refs.
The feasibility was studied of the application of radionuclide X-ray fluorescence analysis to the identification and determination of chemical elements in the air. A description of the method is presented, the main stages of the analysis are discussed (sample preparation and standards, selection of radioactive radiation sources, geometry of measurement and evaluation of results). The method is illustrated on the determination of elements Fe, Cu, Zn, Br, and Pb in air samples taken in the city of Prague. (author) 2 tabs., 2 figs., 14 refs.
Buffer layers with 100% lattice match with YBa2Cu3O7 - ? (YBCO) were prepared from mixed rare-earth-oxides applying a simple sol-gel process and dip-coating method. Structural analysis of the sol-gel derived powder by X-raydiffraction revealed that the mixing parameter, which eliminates the lattice mismatch with YBCO, is x = 0.2382, 0.1852, 0.1252, 0.0906, 0.0793 and 0.0395 in (Eu1 - xHox)2O3, (Eu1 - xErx)2O3, (Eu1 - xYbx)2O3, (Gd1 - xHox)2O3, (Gd1 - xYx)2O3 and (Gd1 - xYbx)2O3, respectively. Microstructural investigations were carried out for Gd1.819Ho0.181O3 films epitaxially grown on cube-textured Ni (100) substrates by sol-gel dip-coating process. X-raydiffraction of the buffer showed strong out-of-plane orientation on Ni tape. The (Gd1 - xHox)2O3 (222) pole figure indicated a single cube-on-cube textured structure. The omega and phi scans revealed good out-of-plane and ...
The structure of ammonium azide (NH{sub 4})N{sub 3} was (re-)determined ab initio from x-ray powder diffraction experiment using synchrotron radiation. We tried to detail and comment the different steps involved in the structure determination. The compound crystallize in the orthorhombic Pmna space group (no.53) with a = 8.937(1) A, b= 3.8070(5) A, c = 8.664(1) A, V = 294.79(7) A{sup 3}; Z= 4. It was possible to locate and refine the hydrogen coordinates, in two different approaches, and to establish the H-bonds. The final structural parameters are in good agreement with previous results based on three-dimensional neutron diffraction. (Author)
The structure of ammonium azide (NH_4)N_3 was (re-)determined ab initio from x-ray powder diffraction experiment using synchrotron radiation. We tried to detail and comment the different steps involved in the structure determination. The compound crystallize in the orthorhombic Pmna space group (no.53) with a = 8.937(1) A, b= 3.8070(5) A, c = 8.664(1) A, V = 294.79(7) A"3; Z= 4. It was possible to locate and refine the hydrogen coordinates, in two different approaches, and to establish the H-bonds. The final structural parameters are in good agreement with previous results based on three-dimensional neutron diffraction. (Author)
We present preliminary analysis for the feasibility of the attosecond x-ray pulses at a proposed FERMI@ELETTRA free electron laser (FEL) [1]. In part 1 we restrict ourselves to minimal modifications to the proposed FEL and consider a scheme for attosecond x-ray production which can be qualified as a small add-on to a primary facility. We demonstrate that at 5-nm wavelength our scheme is capable for production of pulses with an approximate duration of 100 attoseconds at approximately 2 MW peak power and with an absolute temporal synchronization to a pump laser pulse. In part 2 we propose to use an FEL amplifier seeded by a VUV signal and to follow it by the scheme for attosecond x-ray production described in part 1.
A method of kinetic analysis applicable to non-isothermal oxidation processes of ceramic nanocomposites is presented using Ti-Si-C-N powder as the substrate. The nanoparticle size and phase composition were determined using high-resolution transmission electron microscopy and X-raydiffraction (XRD). Thermogravimetric measurements were carried out for powder samples in dry air in the temperature range 298-1770 K. The following heating rates were applied: 3, 5, 10, 20 K min{sup -1}. Mass spectrometry was used to analyze gaseous oxidation products and solid products were identified by the XRD technique. The Coats-Redfern equation was applied for the kinetic analysis. For each stage of the oxidation kinetic models, the best accuracy was achieved using a series of criteria, and then the A and E parameters of the Arrhenius equations were estimated. Both linear regression and artificial neural networks were ...
BaTiO{sub 3} compacts, when fluxed with {lt} 2 vol% of a complex borate glass phase, were sintered to near theoretical density at temperatures {lt} 1175{degrees}C in 2 h. Microstructural analysis showed a uniform grain size {lt} 1.0 {mu}m with 0.75 wt% ZrO{sub 2} added to the flux phase as a grain growth inhibitor. TEM analysis revealed a microcrystalline grain-boundary phase with the ZrO{sub 2} resident along the grain boundaries. These samples displayed an essentially flat dielectric profile, low dissipation factors ({lt} 2%) over the range 25{degrees} to 125{degrees}C, a near linear dependence ({approx} {+-} 15%) between 25{degrees} and {minus} 55{degrees}C, and significantly increased voltage stability. X-raydiffractionanalysis of these small-grained materials indicates a suppression of the tetragonal structure toward a more cubic modification.
BaTiO_3 compacts, when fluxed with < 2 vol% of a complex borate glass phase, were sintered to near theoretical density at temperatures < 1175 degrees C in 2 h. Microstructural analysis showed a uniform grain size < 1.0 #mu#m with 0.75 wt% ZrO_2 added to the flux phase as a grain growth inhibitor. TEM analysis revealed a microcrystalline grain-boundary phase with the ZrO_2 resident along the grain boundaries. These samples displayed an essentially flat dielectric profile, low dissipation factors (< 2%) over the range 25 degrees to 125 degrees C, a near linear dependence (#approx# #+-# 15%) between 25 degrees and - 55 degrees C, and significantly increased voltage stability. X-raydiffractionanalysis of these small-grained materials indicates a suppression of the tetragonal structure toward a more cubic modification.
This thesis is concerned with the optimization and development of the production of nanofocusing refractive X-ray lenses. These optics made of either silicon or diamond are well-suited for high resolution X-ray microscopy. The goal of this work is the design of a reproducible manufacturing process which allows the production of silicon lenses with high precision, high quality and high piece number. Furthermore a process for the production of diamond lenses is to be developed and established. In this work, the theoretical basics of X-rays and their interaction with matter are described. Especially, aspects of synchrotron radiation are emphasized. Important in X-ray microscopy are the different optics. The details, advantages and disadvantages, in particular those of refractive lenses are given. To achieve small X-ray beams well beyond the 100 nm range a small focal length is ...
A galactose-specific seed lectin was purified from the legume Spatholobus parviflorus and crystallized using the hanging-drop vapour-diffusion technique. Thecrystals belonged to space group P1, with unit-cell parameters a = 60.998, b=60.792, c = 78.179-, = 101.32, = 91.38, = 104.32. X-raydiffraction data were collected under cryoconditions (100-K) to a resolution of 2.04- using a MAR image-plate detector system mounted on a rotating-anode X-ray (Cu-K) generator. Molecular replacement using legume-lectin coordinates as a search model gave a tetrameric structure.
Composite nitrides (such as BN, TiN) are widely used in various industrial applications because of their extreme wear and corrosion resistance, thermal and electrical properties. in order to obtain composite materials with these optimal properties, it is important to elucidate whether any chemical reactions occur at nitride/metal interfaces, e.g., those involving BN-Ti/TiN. Materials of interest include the deposition by PVD of Ti and TiN on BN substrates. Some of these systems were then subjected to varying degrees of physical and thermal alteration. Detailed X-ray photoelectron spectroscopy (XPS) has therefore been rendered of these interfaces using cross-sectional display and sputter etching. Resulting structural and morphological features have been investigated with transmission electron microscopy (TEM) and X-raydiffraction (XRD). Diffusion of the nitridation, oxynitride formation and interfacial growth are of general ...
Some aspects of metrological provision of X-ray radiometric analyzers for mineral raw composition and gamma-gamma-logging equipment are considered. Standard samples (SS) based on the phenol-formaldehyde resin with the introduced quantities calculated of element compositions in the form of oxides and salts are described. Principles of metrological provision developed are used when carrying out state acceptance tests of X-ray radiometric analyzer RAL-M-102 ''Ehkran'' and gamma-gamma-logging equipmnt RSK-102. Economic benefit from introduction of an SS set is #approx# 60-100 thousand roubles per year.
Analytic expression is derived for X-ray fluorescence dependence on the particle size of powder and slurry media. The expression is obtained for a model of powder medium containing particles of different size and random distribution in the bulk of the sample. Limiting cases of homogeneous and slurry-like media are considered and expressions for calculation of the fluorescence intensity are derived. The results reasonably match the experiment for binary powder mixtures and thus provide evaluation of the powder particle size on the fluorescence intensity for multicomponent polydisperse powder medium
We have implemented a virtual Young's double slit experiment for hard X-ray photons with micro-fabricated bi-prisms. We observe fringe patterns with a scintillator, and quantify interferograms by detecting X-ray fluorescence from a scanned 30nm Cr metal film. The observed intensities are best modeled with a near-field, Fresnel analysis. The maximum fringe number in the overlap region is proportional to the ratio of real to imaginary parts refractive index of the prism material. The horizontal and vertical transverse coherence lengths at beamline APS 8-ID are measured.
We have described the x-ray optics and beamline performance of the ANL X6B beam line at the NSLS. Considerable flexibility has been built into the beam line to accommodate a wide range of x-raydiffraction, scattering, and spectroscopy experiments with various requirements. We presented selected examples of experimental results and showed that with the high intensity, high energy resolution, high-q resolution, and energy tunability, the X6B beam line has become a versatile facility.
Determination of Mn, Fe, Cu, Zn, Hg, Pb, Br, Se, Rb, Sr and Cd in the medicinal plants by radionuclide X-ray fluorescence analysis (using "2"3"8Pu, "2"4"1Am/Ag and "1"2"5I) is described. (author). 12 refs., 2 tabs.
Heavy metals (Pb, Cd, Mn, Cu, Zn, Fe) were determined in surface waters in the surroundings of the depositories of the mining shrubs in the region of Banska Stiavnica (SR) by radionuclide X-ray fluorescence analysis. Allowed concentrations of the determined metals are exceeded numerously (multiplicity in some cases was 10"3-10"6). (author).
Radionuclide x-ray fluorescence analysis was used for the determination of Y, Ba and Cu in thin high-temperature superconducting films. Atomic emission ICP spectrometry was used to estimate the precision and accuracy of analytical results. Reasonable agreement between both methods was obtained when a polynomial calibration curve was applied. (author) 4 refs.; 4 tabs.
The applicability of the radionuclide X-ray fluorescence analysis (RXFA) for qualitative and quantitative evaluation of environmental plant samples is discussed and examples of determination of Mn, Fe, Ni, Cu, Zn, Pb in samples of apple trees are given. The instrumentation, the standard and sample preparation are also presented.
Fe and Zn were determined in various parts of maize (Zea mays) in dependence on quantity of organic substrate EKOFERT as organic fertilizer in soil, using radionuclide X-ray fluorescence analysis. The increase of quantity of organic substrate EKOFERT in soil causes a decrease of heavy metal concentrations in certain parts of the plant. (author). 4 refs., 1 tab.
A survey is presented of studies dealing with radionuclide X-ray fluorescence analysis (RXFA) of impurities in the air, water, soil, sediments and biological materials, mainly blood, urine, hair, soft tissues and bones. Tabulated are lists of published works on RXFA of the air, water and biological materials. (ES).
SiC-AlN and SiC-SiAlON refractory composites were obtained by means of nitridation of the mixtures of silicon carbide (SiC) powder with a broad granulometric distribution and powders of aluminium (Al) and aluminium-silicon (Al-Si) mixtures. The mixtures of the composition Al-25% Si, Al-50% Si and Al-75% Si were previously prepared by means of 'mechanical alloying' technique. Thermodynamic analysis was accomplished in order to evaluate the viability of SiC-SiAlON and SiC-AlN refractories production by the chosen processing method, and the results confirmed viability of such. Investigation of nitridation of Al and Al-Si powder compacts in order to obtain the AlN and #beta#-SiAlON matrix phases of the composite was accomplished by means of differential thermal analysis (DTA) and thermogravimetric analysis (TG). The results of the thermal analysis show that nitridation of the Al-25% Si, Al-50% Si and Al-75% ...
The possibilities of using both selective heavy ion induced X-ray emission and secondary ion mass spectroscopy (SIMS), for the identification of impurities present at low concentrations in cadmium telluride are examined. The relative concentrations of the impurities along CdTe crystals have been determined by exciting the X-ray emission of the elements in several slices with Ar and Kr ions and by comparing the relative characteristic X-ray emission yields. As a consequence of the quasimolecular inner shell ionization mechanism in heavy ion-atom collisions, Ar and Kr ions allow a strong excitation of the main impurities seen by SIMS namely Si, Cl and Ge, As, with only a minor contribution of Cd and Te. From the changes of the concentrations of the various impurities along the crystal, informations about segregation coefficients and compensation can be obtained.
We present a sample preparation method for measuring magnesium in individual whole lymphocytes by electron probe X-ray microanalysis. We use Burkitt's lymphoma cells in culture as the test sample and compare X-ray microanalysis of individual cells with atomic absorption analysis of pooled cell populations. We determine the magnesium peak-to-local continuum X-ray intensity ratio by electron probe X-ray microanalysis and calculate a mean cell magnesium concentration of 39 +/- 19 mmol/kg dry weight from analysis of 100 cells. We determine a mean cell magnesium concentration of 34 +/- 4 mmol/kg dry weight by atomic absorption analysis of pooled cells in three cell cultures. The mean cell magnesium concentrations determined by the two methods are not significantly different. We find a 10% coefficient of variation for both methods of ...
The formation of textured YBa{sub 2}Cu{sub 3}O{sub 7-{delta}} (123) from a liquid phase according to the peritectic reaction Y{sub 2}BaCuO{sub 5} (211) + liquid {yields} 123 was analyzed using real-time analysis techniques of high-temperature X-raydiffraction, high-temperature optical microscopy, and environmental scanning electron microscopy (ESEM). Results were coupled with conventional ''post-mortem'' SEM analysis of processed samples at various stages of microstructural development. Observations of 123 formation and growth from the peritectic melt permit the conclusion that the presence of crystalline 211 primarily acts as a source of yttrium. The slow dissolution of 211 into the yttrium deficient liquid phase is the rate controlled step in the formation and growth of the textured 123, rather that its acting as a nucleation site for 123 grains as has been widely ...
A test to determine the lithium compatibility and impurity gettering capabilities of various materials including yttrium was performed in Beryllium-7 Experimental Lithium (7BELL) at 270/sup 0/C. Yttrium coupons were exposed in liquid lithium for a total of 3,718 hours. X-raydiffraction and bulk chemical analysis data indicated that yttrium absorbs hydrogen from liquid lithium at 270/sup 0/C and transforms to yttrium dihydride (YH/sub 2/). The transformation of yttrium to YH/sub 2/ resulted in embrittlement of the coupons and subsequent fragmentation to small pieces. Additional analysis, based on the equilibrium hydrogen pressures for the transition of yttrium to YH/sub 2/, and Sievert's relationship for hydrogen in equilibrium with hydrogen in lithium, indicates that the temperature of yttrium cannot exceed 280/sup 0/C to control the hydrogen concentration in lithium at below 1 wt ppm. It is ...
Red mud is a by-product of the alkaline extraction of aluminum from the bauxite and represents a renewed environmental problem due the significant annual throughput by the plants. In the present work, the pozzolanic properties of Brazilian red mud fired at 600, 700, 800 and 900 deg C were investigated by monitoring lime consumption using DTA analysis and Brazilian standard methodology NBR 5772 (1992). Products and kinetics of hydration were determined in cement pastes produced with 5 and 15% red mud using x-raydiffraction and DTA analysis. Compressive strength and capillary absorption tests were realized on mortars constituted by 5, 10 and 15% red mud in replacement of cement. When calcined at 600 deg C, the red mud develops good pozzolanic properties, and the compressive strength of mortars produced with this waste meet values in accordance with regulatory standard. These results shown than red mud ...
Red mud is a by-product of the alkaline extraction of aluminum from the bauxite and represents a renewed environmental problem due the significant annual throughput by the plants. In the present work, the pozzolanic properties of Brazilian red mud fired at 600, 700, 800 and 900 deg C were investigated by monitoring lime consumption using DTA analysis and Brazilian standard methodology NBR 5772 (1992). Products and kinetics of hydration were determined in cement pastes produced with 5 and 15% red mud using x-raydiffraction and DTA analysis. Compressive strength and capillary absorption tests were realized on mortars constituted by 5, 10 and 15% red mud in replacement of cement. When calcined at 600 deg C, the red mud develops good pozzolanic properties, and the compressive strength of mortars produced with this waste meet values in accordance with regulatory standard. These results shown than red mud ...
Si/Ni alloy and graphite composites were synthesized using arc-melting followed by high energy mechanical milling (HEMM). Alloy particles comprising of NiSi2, NiSi and Si phases were distributed finely and uniformly on the surface of graphite in the composites obtained after Hem. The composite containing 60 wt.% of Si/Ni alloy exhibited a stable capacity of ?780 mAh/g. Fourier transform infrared spectroscopy (FTIR) analysis confirmed that some bonds were formed between alloy and graphite after HEMM, which appeared to retain the electrical connection between alloy and graphite during cycling. X-raydiffraction (XRD) analysis indicated that NiSi2 and NiSi phases, which acted as an inactive alloy matrix remained invariant during charge and discharge. In addition to NiSi2 and NiSi phases, disordered graphite layers also played the role of media for the accommodation of large volume change of Si during ...
In this study, perovskite type oxide YAlO_3 has been doped with different amounts of the divalent cation Ca to synthesize Y_1_-_xCa_xAlO_3_-_#delta# (x = 0-0.21) compositions. The effect of dopant concentration on the crystal structure and electrical properties of YAlO_3 synthesized by citrate gel route has been investigated. The phase purity of the samples has been carried out using X-raydiffraction. The microstructural evaluation of the samples has been conducted by scanning electron microscopy and energy dispersive spectrum analysis. Thermal analysis has been conducted to monitor the decomposition of the intermediate products. The electrical conductivity studies have been performed using a.c. impedance spectroscopy as a function of temperature in the range 200-800 "oC in air. The Y_0_._9_4Ca_0_._0_6AlO_3_-_#delta# composition exhibits a total conductivity of 2.5 mS/cm at 800 "oC.
A technique for following sialon formation in situ by high temperature X-raydiffraction (HT-XRD) was developed. The composition chosen for study was an yttrium #alpha#-sialon with x=0.4. Powder compacts containing silicon nitride, aluminum nitride and yttria powders were pre-sintered at 1350 C and then studied by HT-XRD at temperatures between 1450 and 1580 C and nitrogen pressures of 0.11 MPa. The furnace was made from graphite coated with porous silicon nitride/silicon carbide. The coating prevented silicon carbide formation in the sample up to 1600 C. X-raydiffraction results show the formation of a Y_1_0Al_2Si_3O_1_8N_4 phase at 1350 C, which dissolved to form #alpha#-sialon and other phases at higher temperatures. The amounts of #alpha#-sialon formed are similar to the amounts reported by other authors. An empirical method was used for the calculation of activation energy for the silicon nitride ...
The purpose of this research is to investigate the micro-mechanism of deformation behavior of metallic glasses. We report the results of direct observations of short-range and medium-range structural change during tensile deformation of metallic glasses by high energy X-raydiffraction method. Cu50Zr50 and Ni30Zr70 metallic glass samples in the ribbon shape (1.5 mm width and 25 ?m) were made by using rapid quenching method. Tensile deformation added to the sample was made by using special equipment adopted for measuring the high energy X-raydiffraction. The peaks in pair distribution function g(r) for Cu50Zr50 and N30iZr70 metallic glasses move zigzag into front and into rear during tensile deformation. These results of direct observation on atomic distribution change for Cu50Zr50 and Ni30Zr70 metallic glass ribbons during tensile deformation suggest that the micro-relaxations occur.
Five hydrated inorganic divalent cations, Mg[sup 2+], Co[sup 2+], Ni[sup 2+], Cu[sup 2+], and Zn[sup 2+], have successfully been used as templates for the synthesis of manganese oxide octahedral molecular sieves (OMS-1) having the todorokite structure. The OMS-1 samples have been well characterized by X-raydiffraction, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy/energy dispersive X-ray studies, inductively coupled plasma analysis, electron paramagnetic resonance, Fourier transform infrared spectroscopy, thiosulfate titration, and cyclohexane sorption. Catalytic CO oxidation and 2-propanol decomposition were carried out. Results show that these OMS-1 samples with a tunnel size of about 6.9 angstroms are crystalline and chemically pure. They have the following formulas: Mg[sub 3.17]Mn[sub 5.05]O[sub 12] [center dot] 4.52H[sub 2]O, ...
It is shown that it is necessary to take into account locality of the analysis and to introduce additional corrections for partial capture of matrix and fluorescent subexcitation by matrix during quantitative X-ray spectral microanalysis of finely dispersed materials. Cast two-phase (#alpha#+#beta#) titanium alloy VT3-1 is chosen as an investigation object.
Radiometric X-ray fluorescence analysis was used for the determination of Mn, Fe, Cu, Zn and Pb in wastewater and sludges from three wastewater treatment plants in Bratislava (SR). Metals were determined in wastewaters after preconcentration by 8-hydroxyquinoline and in sludges by drying and pressing to pellets. "2"3"8Pu and "1"0"9Cd was used for excitation of fluorescence radiation. (author).
Radionuclide X-ray fluorescence analysis was used for the determination of Cr, Fe, Cu, Zn and Ph in industrial wastewaters (from surface treatment of metals and glasses) after precipitation of determined elements by 8-hydroxyquinoline. (author).
ORNL has developed the technology to detect hidden explosives in luggage using Xray and neutron detection devices. The Federal Aviation Administration has ordered the airlines to buy and install Thermal Neutron Analysis (TNA) units. The combined pulsed-neutron and X-ray interrogation inspection (CPNX) system developed at ORNL uses less radioactive materials as well as being more sensitive to weapons, electronic devices and plastic explosives.
Radionuclide x-ray fluorescence method was used in the determination of Cr, Ni and other heavy metals content in wastewater of an engineering plant taken both before and after chemical treatment. Toxic effects of the wastewaters using Allium cepa root tip cells were tested. (author) 8 refs.; 2 tabs.
A radiometric method was elaborated for surface density determinations of the adhesive layer of plasters by radionuclide X-ray fluorescence using the 17.47 keV bremsstrahlung of "1"4"7Pm/Mo. The bremsstrahlung line excites the 8.63 keV characteristic K#alpha# line of Zn contained in the adhesive layer of the plaster as a filling material in the form of ZnO. In homogeneous adhesive layers the Zn content is proportional to surface density. (author).
Radionuclide X-ray fluorescence method was used for the determination of Fe and Zn in healing plants (Sage, Peppermint, Stinging, Common Agrimony, Milfoil, Ribwort, Tansy, White Dead-Nettle). "2"3"8Pu exciting source and Si/Li semiconductor detector were used for the determination. (author)
Radionuclide X-ray fluorescence method with Si/Li semiconductor detector and "2"3"8Pu exciting source was used for the determination of Cu, Ni, Zn and Pb in plant samples (Taraxacum officinale) from various localities near the highway D-61 Bratislava-Trnava (SR). (author) 2 refs.; 1 fig.; 1 tab.
Radionuclide X-ray fluorescence method with Si/Li semiconductor detector and "2"3"8Pu exciting source was used for the determination of Cu, Ni, Pb, and Zn in soil samples from various localities near the D-61 Bratislava-Trnava highway (CSFR). (author) 1 ref.; 1 tab.
An energy dispersive x-ray fluorescence technique was used for the determination of Titanium (Ti) and Zirconium (Zr) in red mud by using a standard addition method. An annular {sup 241}Am source is employed for excitation of K shells of elements. 13 refs., 2 figs., 1 tab.
As thin films become increasingly popular (for solar cells, LEDs, microelectronics, batteries), quantitative morphological information is needed to predict and optimize the film's electronic, optical and mechanical properties. This quantification can be obtained quickly and easily with X-raydiffraction using an area detector and synchrotron radiation in two simple geometries. In this paper, we describe a methodology for constructing complete pole figures for thin films with fiber texture (isotropic in-plane orientation). We demonstrate this technique on semicrystalline polymer films, self-assembled nanoparticle semiconductor films, and randomly-packed metallic nanoparticle films. This method can be immediately implemented to help understand the relationship between film processing and microstructure, enabling the development of better and less expensive electronic and optoelectronic devices.
High-energy synchrotron x-raydiffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.
Wood plastic composite (WPC) of kadom, simul, mango and debdaro were prepared with two monomers methylmethacrylate (MMA) and butylmethacrylate (BMA) using high energy ionizing radiation. X-raydiffraction and scanning electron microscope (SEM) studies reveal that significant grafting occurred with wood fiber. Electric properties like resistivity and dielectric constant of both wood and WPC were measured under different moisture contents and relative humidities. The resistivities of wood decreased dramatically with increase of moisture content, but those of WPC decreased very slowly with moisture content. The dielectric constant of wood increased significantly with moisture content but no significant difference was observed in the case of WPC within the range of moisture contents studied. The dielectric constants of untreated wood also increased with their densities. (author).
The elemental and mineralogical variation in a self-burning coal seam from Coalspur, Alberta, is determined using instrumental neutron activation analysis (INAA) and x-raydiffraction (XRD). The elemental variation in the coal seam is related to temperatures in the various alteration zones, i.e., oxidation, combustion, or carbonization and nature of elements. Mobilization of elements is greatest for As, Br, Cl, Mo, N, S, and Sb. Some of these elements are released to the atmosphere, as evident by the presence of orthorombic sulfur crystals on the surface or in vents at the top of the burning seam or saturation of oxidation char by volatile matter (tar). Whewellite (CaC{sub 2}O{sub 4}, H{sub 2}O) is the only Ca-bearing mineral found in the cooler area of the coal seam. Decomposition of this mineral, coupled with the presence of SO{sub 2} formed by reaction of organic sulfur with O{sub 2} in combustion, resulted in formation ...
An alternative to synthetic materials for use in solar pond liners is to select clayey soils as hydraulic barriers. This option reduces the cost of construction and the risk of contamination of subsoil and groundwater by hot brines. This paper deals with the physical, chemical and hydraulic properties of different soils tested mainly as compacted clay liners. The underdeveloped nations have the option to use this type of liner, but before doing so several tests are recommended, including those for soil and water composition, permeability, plasticity and X-raydiffractionanalysis. In this investigation the following samples are analyzed: native clayey soils with illite, montmorillonite and halloysite, treated and non-treated bentonites in powder and granulated form, a mixture of zeolite and sodium bentonite, and industrial minerals composed largely of halloysite, kaolinite and attapulgite selected clays. Neutral salt ...
The crystallite size and orientation in molybdenum films prepared by magnetron sputtering at a low rate of typical 1 (angstrom)s and a pressure of 0.45 Pa was investigated by X-raydiffraction and texture analysis. The surface topography was studied using atomic force microscopy. Increasing the film thickness from 20 nm to 3 microm, the films show a turnover from a (110) fiber texture to a (211) mosaic-like texture. In the early state of growth (20 nm thickness) the development of dome-like structures on the surface is observed. The number of these structures increases with film thickness, whereas their size is weakly influenced. The effect of texture turnover is reduced by increasing the deposition rate by a factor of six, and it is absent for samples mounted above the center of the magnetron source. The effect of texture turnover is related to the bombardment of the films with high energetic argon neutrals resulting from ...
Mixed-conducting Sr-Fe-Co oxides have potential applications in dense ceramic membranes for high-purity oxygen separation and/or methane conversion to produce syngas (CO + H{sub 2}), because of their combined high electronic/ionic conductivity and significant oxygen permeability. We studied the crystal structure and microstructure of the system in X-raydiffraction experiments and by using scanning electron microscopy, respectively. Thermogravimetric analysis was conducted on the SrFeCo{sub 0.5}O{sub x} sample in environments of various oxygen partial pressures (pO{sub 2}). Conductivity increased while weight decreased with increasing temperature. Activation energy decreased while conductivity increased with increasing pO{sub 2}. The pO{sub 2}-dependent conducting behavior of the SrFeCo{sub 0.5}O{sub x} system can be understood by considering the trivalent-to-divalent transition of transition-metal ions.
Sintered glass-ceramics were produced from coal fly ashes, red mud from aluminum production and silica fume. The capabilities of Tuncbilek fly ash and a mixture of Orhaneli fly ash, red mud and silica fume to be vitrified and devitrified by sintering process were investigated by means of scanning electron microscopy and X-raydiffractionanalysis. To determine the effect of binder in the sintering technique, glass powders were pressed without or with the addition of polyvinyl alcohol. Owing to microstructural observations, density and hardness measurements, it can be said that physical properties and the hardness of the produced samples strongly depended on the crystallization degree of the samples. Toxicity characteristic leaching procedure test results showed that glass-ceramic samples produced by using sintering technique could be considered as nonhazardous materials. Chemical durability of the sintered glass-ceramic ...
A WO3/TiO2 composite, hollow-sphere photocatalyst with average diameter of 320nm and shell thickness of 50nm was successfully prepared using a template method. UV-vis diffuse reflectance spectra illustrated that the main absorption edges of the WO3/TiO2 hollow spheres were red-shifted compared to the TiO2 hollow spheres, indicating an extension of light absorption into the visible region of the composite photocatalyst. The WO3 and TiO2 phases were confirmed by X-raydiffractionanalysis. BET isotherms revealed that the specific surface area and average pore diameter of the hollow spheres were 40.95m^2/g and 19nm, respectively. Photocatalytic experiments indicate that 78% MB was degraded by WO3/TiO2 hollow spheres under visible light within 80min. Under the same conditions, only 24% MB can ...
Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitatively low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed the crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size ...
The X-raydiffractionanalysis of (U,Ce)O{sub 2} with the CeO{sub 2} contents ranging from 0 to 20 mol% CeO{sub 2} was performed at room temperature to obtain the variation in the lattice parameter with the CeO{sub 2} content. Ultrasonic pulse echo measurements were also carried out to estimate the change in the mechanical properties of (U,Ce)O{sub 2} with the CeO{sub 2} content. The lattice parameter of (U,Ce)O{sub 2} was found to decrease with increasing CeO{sub 2} content. The variation in the lattice parameter with the CeO{sub 2} content closely followed the Vegard law. The shear and longitudinal velocities in (U,Ce)O{sub 2} were found to decrease with increasing CeO{sub 2} content. The Young`s and shear moduli, and Poisson`s ratio estimated from the wave velocities decreased with the CeO{sub 2} content. No mechanical property showed anomaly in low CeO{sub 2} content region. (orig.).
Potassium dichlorido(l-prolinato)platinate(II), K[PtCl"2(l-pro"?"H)] (1), and chlorido(dimethyl sulfoxide)(l-prolinato)platinum(II), [PtCl(l-pro"?"H)(dmso)] (2), were synthesized by ligand substitution reactions. Both complexes were characterized by ^1H, ^1^3C, and ^1^9^5Pt NMR spectroscopy, elemental analysis, and HR-ESI-MS. The molecular structures of 1 and 2 were determined by single crystal X-raydiffraction, proving bidentate coordinated l-prolinato ligand and SP-4-4 configuration of 2a. With the help of DFT calculations stability of possible isomers of 1 and 2 was studied. A considerable difference in the in vitro cytotoxicity of 1 versus 2a (exchange of one chlorido ligand by dmso) against four human cancer cell lines was found.
The structure and vibrational properties of high voltage cathode materials, namely LiNi{sub 1-y}CO{sub y}VO{sub 4} solid solution with (0{<=}y{<=}1), have been studied using X-raydiffraction, Raman scattering and FTIR measurements. Rietveld refinements show that LiNi{sub 1-y}Co{sub y}VO{sub 4} vanadates belong to the inverse spinel structure with Fd3m(O{sup 7}{sub h}) space group. Analysis of Raman spectra has been carried out in the molecular approximation using a local environment model including VO{sub 4} tetrahedra, (Ni, Co)O{sub 6} and LiO{sub 6} octahedra as vibrational local units. (orig.)
Stearic acid gel is employed to study the phase evolution of MgTiO{sub 3} nanoparticles by thermal gravimetric analysis, X-raydiffraction, and Fourier transform infrared. During the preparation of stearic acid gel, tetrabutyl titanate easily absorbed moisture to hydrolyze into Ti(OH){sub 4} firstly, and then reacts with stearic acid and magnesium stearate to form magnesium-titanium oxide network polymer gel, meanwhile n-butanol is generated. When stearic acid gel is calcined in air, a series of oxidation and combustion reactions occur, meanwhile apparent heat is given off. The results show that a metastable intermediate phase Mg{sub 2}TiO{sub 4} is generated at 450 {sup o}C and nearly disappeared at 550 {sup o}C. Simultaneously, a new solid phase of MgTiO{sub 3} appears. The metastable intermediate phase Mg{sub 2}TiO{sub 4} is successfully identified in the current work.
Microhardness decarburization profiles are often used in the industry to estimate the carbon distribution in steels. For quantitative evaluation, an analysis based on diffusion theory must be performed, the fundamentals and mathematical basics of which are presented. If the relationship between hardness and carbon content is known, microhardness-distance curves of steels can be analyzed in this way. For martensitic grades, for instance, a linearized expression holds in the concentration range from 0.15 to 0.6 m.% C. Microhardness depth profiles of higher carbon steels and other microstructures, however, are also evaluated in the literature. The applicability of quantitative diffusion modeling is discussed in detail. Through hardenable rolling bearing steel 100Cr6 (1.3505, SAE 52100) serves as model material: carbon concentration-distance curves are measured with high accuracy by secondary ion mass spectrometry (SIMS) and compared with microhardness decarburization ...
The present investigation deals with the fabrication of liquid petroleum gas (LPG) sensor based on semiconducting oxide SnO{sub 2}. The gas sensor elements have been prepared by conventional solid state route. Addition of noble metal sensitizer, palladium and grain growth inhibitor, aluminum silicate to the base material SnO{sub 2}, not only improved the sensitivity towards LPG but also the selectivity in the presence of CO and CH{sub 4} gases. Out of various sensor compositions, SnO{sub 2}:Al{sub 2}Si{sub 2}O{sub 7} (35 wt.%):Pd (1.5 wt.%) sintered at 800 C for 5 h has shown high sensitivity (0.97) towards LPG at an operating temperature of 350 C. Different characterization techniques have been employed, such as differential thermal analysis (DTA), surface area analyzer, X-raydiffraction (XRD), to study the formation of SnO{sub 2}, surface area and crystallite size, respectively. The results suggested the possibility of ...
The Si_3N_4-rich corner of the phase diagrams for neodymia and ytterbia containing sialons has been investigated by a systematic variation of the m and n values for compositions between 0.5 and 2.0 with a step size of 0.5. Samples requiring nitrides of the rare earth elements have not been prepared. Sintering has been performed at 1800 C for one hour in a nitrogen atmosphere of 1 MPa. The sintered samples were characterized by X-raydiffractionanalysis to identify the crystalline phases in equilibrium with sialon. #alpha#- and #beta#-sialon, the 21R AlN polytypoid, and N-melilite M' were found in the Nd containing system. Materials with Yb showed the formation of #alpha#- and #beta#-sialon, and the AlN polytypoids 12H and 21R. The m and n values of the #alpha#-sialon phase have been calculated via their lattice parameters that were refined by a least squares routine. The occurrence and composition of the phases were used ...
New palladium(II) and platinum(II) complexes of saccharinate (sac), trans-[Pd(py)"2(sac)"2] (1), cis-[Pt(py)"2(sac)"2] (2), trans-[Pd(3-acpy)"2(sac)"2] (3) and cis-[Pt(3-acpy)"2(sac)"2] (4) (py=pyridine and 3-acpy=3-acetylpyridine) have been synthesized. Elemental analysis, UV-Vis, IR, NMR and TG/DTA characterizations have been carried out. The structures of 1-4 were determined by X-raydiffraction. The palladium(II) and platinum(II) ions are coordinated by two N-bonded sac ligands, and two nitrogen atoms of py or 3-acpy, forming a distorted square-planar geometry. The palladium(II) complexes (1 and 3) are trans isomers, while the platinum(II) complexes (2 and 4) are cis isomers. The mononuclear species in the solid state are connected by weak intermolecular C-H...O hydrogen bonds, C-H...@...
The mobility of metals in ground water is an important consideration for evaluating remedial options at the Asarco smelter site. Tacoma, Washington. One factor in assessing metal mobility is the degree of secondary mineralization in a slag-fill aquifer extending into the intertidal zone along the Puget Sound shoreline. Samples of aquifer material were collected for mineralogical analysis from borehole MW-206 at five-foot intervals within the slag fill from 5 to 25 feet below the ground surface, and in the underlying marine sand and gravel at 27 feet. Grab samples of slag fragments with visually apparent secondary minerals were also collected at five intermediate depths between 12 and 19 feet. Samples were analyzed by a variety of techniques including hydride generation/atomic absorption for arsenic concentration, scanning electron microscopy/electron microprobe for mineralogical texture and microanalysis, powder x-ray ...
Experiments on manganese removal using an aerated granular filter with mean particle size of 3.68 mm and 5.21 mm anthracite were conducted at a filtration rate of 100 m d{sup -1}. Air, with a rate of 0 to 366 m d{sup -1}, was supplied through nozzles positioned 100 mm above the filter column bottom. From the experiments that were conducted, it was found that manganese removal is completed at a pH of 9.6 or above. In addition, the oxidation and removal rate of dissolved manganese were expressed as a first-order reaction. The smaller the filter media particles were, the higher the manganese removal efficiency was. The aeration rate of dissolved oxygen in raw water is sufficient for the manganese removal process. The manganese removal rate increased with time due to the catalytic effect of manganese dioxide (MnO{sub 2}) attached to the media. The x-raydiffractionanalysis showed that the solids attached to the filter media ...
Mn{sub 1-x}Fe{sub x}In{sub 2}S{sub 4} spinel compounds (x=0.3, 0.8) were grown by the chemical vapor transport method. The analysis of the X-raydiffraction data suggest that both the compounds crystallize in a cubic structure under the space group Fd3m. The magnetic study done between 300 and 2 K showed a paramagnetic behavior for the intermediate concentration sample x=0.3. A good fitting to the Curie-Weiss law allows us to calculate the paramagnetic Curie temperature. They are negative indicating predominant antiferromagnetic interactions. However, in sample with high Fe concentration, x=0.8, it was possible to observe a peak at around T{sub sg} congruent with 10 K. From ac magnetic susceptibility data at different driving frequencies f, it is found that the peak at T{sub sg} shifts to lower temperatures with decreasing frequency suggesting an spin-glass behavior.
For the development of high ionic conductive solid electrolyte, LiTi2(PO4)3 (LTP), one of the promising inorganic solid electrolyte, was synthesized to investigate an effect of additional lithium salt on the ion conductivity. Lithium salt added LTP composite electrolyte sintered at 900{degree}C exhibited highest conductivity, which was two order magnitude higher than pure LTP. Effects of lithium salt addition are as follows. Conductivity of the composite electrolyte provided larger sintering temperature dependence than the pure LTP. From X-raydiffractionanalysis, structures and compositions were resemble between two composite electrolytes. Byproducts except LTP provided rather low conductivity. It was suggested that melted constitution in the composite can affect the sintering improvement by the additional lithium salt at temperatures over 800 {degree}C. From the observation of ruptured surface of sintered specimens, ...
The effects of the plasma nitriding with the formation of compound nitride and diffusion zones and of the boronising with the different ion doses on hydrogen distribution and hydrogen induced deterioration of a surface layer were examined in the case of Armco iron. Electrochemical studies of hydrogen permeation rate, hydrogen vacuum extraction measurements, optical and scanning microscopy, X-raydiffraction and elastic recoil detection analysis (ERDA) were used. Accumulation of entering hydrogen within the various constituent zones of the modified layer inhibits the hydrogen transport into the metal and thus, decreases the mean hydrogen content in the deeper zones and in the core. Hydrogen accumulation within the compact nitride zone causes the expansion of the nitride lattice, nitride phase transformation and deterioration. The ion boronising enhances the hydrogen effects in the plasma nitrided layers. Therefore, ...
The electrochemical method has been used to deposit zinc oxide (ZnO) thin films from aqueous zinc nitrate solution at 80 deg. C onto fluorine doped tin oxide (FTO) coated glass substrates. ZnO thin films were grown between - 0.900 and - 1.025 V vs Ag/AgCl as established by voltammogram. Characterisation of ZnO films was carried out for both as-deposited and annealed films in order to study the effect of annealing. Structural analysis of the ZnO films was performed using X-raydiffraction, which showed polycrystalline films of hexagonal phase with (002) preferential orientation. Atomic force microscopy was used to study the surface morphology. Optical studies identified the bandgap to be {approx} 3.20 eV and refractive index to 2.35. The photoelectrochemical cell signal indicated that the films had n-type electrical conductivity and current-voltage measurements showed the glass/FTO/ZnO/Au devices exhibit rectifying ...
Flow-curve characteristics of the heat-resistant steels X 20 CrMoV 12.1 and alloy 800 (X5NiCrTiAl32.20) were measured by tensile and compression tests at temperatures between room temperature and 800 C and strain rates {epsilon}{<=}10 s{sup -1} in connection with microstructure investigations (dislocation content, carbide precipitation) by TEM and X-raydiffractionanalysis (XDA). Modelling the deformation behaviour of the steels in terms of the microstructure development indicates that it cannot be explained in a simple manner. The flow curves {sigma}={sigma}({epsilon}, {epsilon}, T) lie, in general, between those predicted by the Kocks-Mecking-Estrin model and a modified (i.e. two-parameter) Roberts model. Because of the less complicated nature of the deformation process the correspondence of experiment and modelling is more satisfying in the case of the material X 20 CrMoV 12.1. (orig.) 26 refs.
The total hemispherical emittance of an oxide film that formed on 6061-T6 aluminium alloy parts in the Tower Shielding Reactor-II at Oak Ridge National Laboratory was measured from 295 to 773 K using an emissometer and/or a calorimeter. The emittance of this film was critically needed for heat transfer calculations in a simulated loss-of-coolant accident of the reactor. X-raydiffractionanalysis identified the film as boehmite (Al{sub 2}O{sub 3} {times} H{sub 2}O), which dehydrated to alumina (Al{sub 2}O{sub 3}) upon heating above 473 K. The measured emittances for the alumina film are in excellent agreement with published values for anodized aluminum films and for bulk alumina. Published values of the emittance of boehmite could not be found for comparison, but evidence is presented that some anodization processes for aluminum yield boehmite and not alumina films.
In this study, Cu{sub 2}O/Cu composite particles were synthesized using an innovative chemical reduction method without any template and surfactant. X-raydiffraction (XRD) analysis revealed that the product mainly consisted of Cu{sub 2}O phase coexisting with a Cu phase. FE-SEM images showed that the octahedral shaped particles were Cu{sub 2}O. The electrochemical performance of the Cu{sub 2}O/Cu particles was investigated with regards to the working electrode material in alkaline solution. The particles had a maximum discharge capacity of 222.9 mAh/g at a discharge current density of 60 mA/g and a high value of 109.1 mAh/g after 50 charge-discharge cycles. Cyclic voltammetry revealed that the reaction between Cu{sub 2}O and Cu is the major electrochemical reaction during the charging and discharging process. Electrochemical impedance spectroscopy revealed that the formation of Cu{sub 2}O on the surface of Cu particles ...
BaxSr1-xTiO3 (x=0.6, 0.75, 0.80, 0.85 and 0.9) compositions are prepared by solid-state reaction route using controlled heating and cooling. Density optimization by varying sintering temperature was achieved. X-raydiffraction (XRD) analysis shows the phase pure materials. The lattice constant decreases from 3.9868A (x=0.90) to 3.9449A (x=0.60) with increasing Sr2+; the tetragonal distortion also decreases. Dielectric constant show sharp peaks for samples having low strontium content (0.10, 0.15) and gets smeared out as the strontium content is increased (0.20, 0.25). For further higher Sr2+ composition (0.40), the dielectric peak could not be observed in the measured temperature range. The peak broadening in Sr2+ rich compositions indicates that diffused transitions and is attributed to t...
The properties of polycrystalline (Ti, Al)N coatings deposited on non-nitrided, classically plasma-nitrided and low pressure plasma-nitrided AISI H11 steel samples were investigated. The plasma deposition and low pressure plasma nitriding were performed in a Z700-LH magnetron sputter ion plating unit, while a separate unit was used for plasma nitriding of specimens at a pressure of several millibars. The (Ti, Al)N coating was deposited onto all the samples using the same equipment as for the plasma deposition and low pressure plasma nitriding. For the characterization of the composite structures, the following methods were used: scratch test, X-raydiffractionanalysis, scanning electron microscopy, scanning tunnelling microscopy and microhardness testing. It was found that plasma nitriding prior to coating deposition strongly affects the growth and properties of hard coatings, such as the microhardness, adhesion, preferred ...
A Ni3Al coating was prepared by plasma spraying technique on the surface of titanium alloy. Ni-Al mixed powders, coatings and reaction products were investigated by scanning electron microscope, EDS, DSC and XRD. A tight bonding between the coating and the substrate was formed. The X-raydiffractionanalysis of the patterns showed that the coating not only had Ni3Al phase, but also had NiO and Al2O3 phase microcontent. Comparing Ni coated Al to Ni3Al at 900^oC, the diffusion was stronger and the diffusion layer was thicker. A minute pore structure was formed at 1200^oC in the front edge of solid-state reaction layer. So Ni3Al restrained the solid-state reaction of the coating with the substrate, and as a whole weakened the entry of oxygen atoms into the substrate and quenched the out-diffu...
SiAlONs are ceramics with high potential as biomaterials due to their chemical stability, associated with suitable mechanical properties, such as high fracture toughness and fracture resistance. The objective of this work was to investigate the mechanical properties and the cytotoxicity of these ceramic materials. Three different compositions were prepared, using silicon nitride, aluminum nitride and a rare earth oxide mixture as starting powders, yielding Si_3N_4-SiAlON composites or pure SiAlON ceramics, after hot-pressing at 1750 deg. C, for 30 min. The sintered samples were characterized by X-raydiffractionanalysis (XRD) and scanning electron microscopy (SEM). Furthermore, hardness and fracture toughness were determined using the Vicker's indentation method. The biological compatibility was evaluated by in vitro cytotoxicity tests. Ceramic with elevated hardness, ranging between 17 and 21 GPa, and high fracture ...
NaCl doped MgCl_2.nEtOH adducts were prepared by ball-milling MgCl_2.2.5EtOH with NaCl. Both the ball-milled MgCl_2.nEtOH/NaCl mixture and pure MgCl_2.2.5EtOH adducts were analyzed by X-raydiffraction (XRD), transmission electron microscope (TEM), thermogravimetry (TG) and differencial scanning calorimetry (DSC). A simple MgCl_2.nEtOH/NaCl mixture without ball-milling treatment was also studied for comparison. Two kinds of mixed crystals, Na_2MgCl_4 and NaMgCl_3, were found to be formed in a ball-milled mixture that contained 16 mol.% NaCl. TG and DSC analysis of the samples also provided indirect evidences supporting the presence of the mixed crystals in the ball-milled mixture. Adding certain amounts of NaCl in MgCl_2.2.5EtOH adduct, either by co-milling or by simple mixing, greatly increased the thermal stability of the adduct, but thermal decomposition behaviour of the ball-milled mixture was still different from that ...
The transport properties of a 'thin' polycrystalline diamond film are analyzed after the sample exposure to 8.06-keV x-ray radiation. Structure and morphology of the as-grown film have been evaluated by Raman, x-raydiffraction, and scanning electron microscopy techniques. The transport properties have been investigated by measuring dark current-voltage characteristics in the temperature range of 60 to 360 K. Ohmic transport has been evidenced on the as-grown film up to 1.16x10"5 V/cm. After irradiation, nonlinear contributions to the dark current have been evidenced and related to field-assisted thermal ionization of traps. Below 200 K, hopping mechanisms have been observed. Correlations have been found among x-ray irradiation, density of traps involved in the transport processes, and the nonhomogeneous nature of the sample. A simple model of the grain boundary structure is proposed to explain the ...
Porous nanostructured LiFePO{sub 4} powder with a narrow particle size distribution (100-300nm) for high rate lithium-ion battery cathode application was obtained using an ethanol based sol-gel route employing lauric acid as a surfactant. The synthesized LiFePO{sub 4} powders comprised of agglomerates of crystallites <65nm in diameter exhibiting a specific surface area ranging from 8m{sup 2}g{sup -1} to 36m{sup 2}g{sup -1} depending on the absence or presence of the surfactant. The LiFePO{sub 4} obtained using lauric acid resulted in a specific capacity of 123mAhg{sup -1} and 157mAhg{sup -1} at discharge rates of 10C and 1C with less than 0.08% fade per cycle, respectively. Structural and microstructural characterization were performed using X-raydiffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) with energy dispersive X-ray (EDX) ...
In order to understand the chemistry of altermetal dopants in antimony oxide, the detailed structural characterization of two ..beta..-Sb/sub 2/O/sub 4/ compounds is reported, Mo-doped ..beta..-Sb/sub 2/O/sub 4/ (1.5 metal%) and V-doped ..beta..-Sb/sub 2/O/sub 4/ (5 metal%). The methods used to characterize these materials are X-ray and neutron diffraction, scanning electron microscopy, Mo K-edge extended X-ray absorption fine structure spectroscopy, and elemental analysis. The atomic position of each of these dopants in Sb/sub 2/O/sub 4/ is radically different as is the overall effect on the host structure. Molybdenum does not substitute for Sb atoms, rather the Mo atoms are found in channels of electron density formed by Sb/sup 3 +/ lone pairs. The two nearest Sb/sup 3 +/ are absent and the oxygen stoichiometry is preserved. The formula is Sb/sub 1.97/Mo/sub 0.015/O/sub 4/. Vanadium incorporates ...
In this work, {beta}-SnS{sub 2} thin films have been prepared on glass substrates by the spray pyrolysis technique using an alcohol solution which contains tin chloride (SnCl{sub 4}) and thiourea (SC(NH{sub 2}){sub 2}) as precursors. The structural study shows that {beta}-SnS{sub 2} thin film prepared using optimal experimental conditions: substrate temperature T{sub s} = 280 deg. C and the concentration ratio of sulfur and tin elements in the spray solution x = [S]/[Sn] = 2.5, crystallizes in the hexagonal phase with a strong (0 0 1) X-raydiffraction line. In the same way, microprobe analyses (EPMA) as well as X-ray photoelectron spectroscopy (XPS) show the presence of undiserable phase of SnO{sub 2}. From the transmission and reflectance spectra, the band gap energy is 2.65 eV. On the other hand, the photothermal properties of such films have been studied, the thermal conductivity was K{sub c} = 0.85 W m{sup -1} K{sup ...
In this work, ?-SnS2 thin films have been prepared on glass substrates by the spray pyrolysis technique using an alcohol solution which contains tin chloride (SnCl4) and thiourea (SC(NH2)2) as precursors. The structural study shows that ?-SnS2 thin film prepared using optimal experimental conditions: substrate temperature Ts = 280 deg. C and the concentration ratio of sulfur and tin elements in the spray solution x = [S]/[Sn] = 2.5, crystallizes in the hexagonal phase with a strong (0 0 1) X-raydiffraction line. In the same way, microprobe analyses (EPMA) as well as X-ray photoelectron spectroscopy (XPS) show the presence of undiserable phase of SnO2. From the transmission and reflectance spectra, the band gap energy is 2.65 eV. On the other hand, the photothermal properties of such films have been studied, the thermal conductivity was Kc = 0.85 W m-1 K-1 and the thermal diffusivity was Dc = 14.5 x 10-6 m2 s-1. The ...
I present an exact calculation of free-electron-laser (FEL) eigenmodes (fundamental as well as higher order modes) in the exponential-gain regime. These eigenmodes specify transverse profiles and exponential growth rates of the laser field, and they are self-consistent solutions of the coupled Maxwell-Vlasov equations describing the FEL interaction taking into account the effects due to energy spread, emittance and betatron oscillations of the electron beam, and diffraction and guiding of the laser field. The unperturbed electron distribution is assumed to be of Gaussian shape in four dimensional transverse phase space and in the energy variable, but uniform in longitudinal coordinate. The focusing of the electron beam is assumed to be matched to the natural wiggler focusing in both transverse planes. With these assumptions the eigenvalue problem can be reduced to a numerically manageable integral equation and solved exactly with a kernel iteration method. An ...
Shocked quartz minerals from the Cretaceous-Tertiary (K/T) boundary and impact craters have been mainly discussed from distribution of optical directions, mean optical refractive index, and X-ray data (1). The purpose of the present study is presentation of the detailed mineralogical data of shocked quartz found in the K/T boundaries and terrestrial impact craters (2,3,4,5). X-ray powder diffraction pattern of shocked quartz aggregate reveals that all Xray peaks are split into major three peaks composed of low-density quartz (LQ), normal quartz (Q), and shocked quartz with high density (SQ). X-ray peaks of (110), (200), (201), (202), and (211) in the hexagonal cell are also split into many peaks. The X-ray intensity among LQ, Q, and SQ phases indicates that the SQ phase shows 36% to 53% in six K/T boundary samples (5). The relative X-ray intensity ratio of ...
We have performed X-ray magnetic diffraction (XMD) experiment of ferromagnets at the Photon Factory (PF) of the High Energy Accelerator Research Organization (KEK) in Tsukuba. In this study, we have upgraded the XMD experimental system in order to apply this method to as many samples as possible. Upgrade was made for (1) the X-ray counting system and related measurement program, (2) the electromagnet, and (3) the refrigerator. The performance of the system was enhanced so that (1) the counting rate capability was improved from 104cps to 105cps, (2) the maximum magnetic field was increased from 0.85T to 2.15T, and (3) the lowest sample temperature was reduced from 15K to 5K. The new system was applied to an orbital ordering compound of YTiO3, and we obtained spin magnetic form factor for the reflection plane (010) perpendicular to the b axis. The magnetic field of 2T was needed to saturate the magnetization of YTiO3 along ...
In this work we report a study of the induced changes in structure and corrosion behavior of martensitic stainless steels nitrided by plasma immersion ion implantation (PI"3) at different previous heat treatments. The samples were characterized by x-raydiffraction and glancing angle x-raydiffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, and potentiodynamic measurements. Depending on the proportion of retained austenite in the unimplanted material, different phase transformations are obtained at lower and intermediate temperatures of nitrogen implantation. At higher temperatures, the great mobility of the chromium yields CrN segregations like spots in random distribution, and the #alpha#"'-martensite is degraded to#alpha#-Fe (ferrite). The nitrided layer thickness follows a fairly linear relationship with the temperature and a parabolic law with the ...
X-ray imaging using asymmetric Bragg reflection in the hard x-ray regime opens the way to improve the spatial resolution limit below 1 #mu#m by magnifying the image before detection, simultaneously providing a strong phase contrast. A theoretical formalism of the imaging process is established. Based on this algorithm, numerical simulations are performed and demonstrate that both Fresnel propagation and Bragg diffraction contribute to contrast formation. The achievable resolution of this technique is investigated theoretically; the results obtained can be used to improve future experimental setups. Furthermore, the minimum detectable phase gradient is estimated, for comparison with other phase sensitive imaging techniques. Results from biological objects demonstrate that the technique is viable for imaging both in two and three dimensions. Refraction contrast images are extracted from experimental projection images by an ...
Particularly high coherence of the x-ray beam is associated, on the ID19 beamline at ESRF, with the small angular size of the source as seen from a point of the sample (0.1-1 #mu#rad). This feature makes the imaging of phase objects extremely simple, by using a 'propagation' technique. The physical principle involved is Fresnel diffraction. Phase imaging is being simultaneously developed as a technique and used as a tool to investigate light natural or artificial materials introducing phase variations across the transmitted x-ray beam. They include polymers, wood, crystals, alloys, composites or ceramics, exhibiting inclusions, holes, cracks, ... . 'Tomographic' three-dimensional reconstruction can be performed with a filtered back-projection algorithm either on the images processed as in attenuation tomography, or on the phase maps retrieved from the images with a reconstruction procedure similar to that used for electron ...
We present a sample preparation method for measuring magnesium in individual whole lymphocytes by electron probe X-ray microanalysis. We use Burkitt's lymphoma cells in culture as the test sample and compare X-ray microanalysis of individual cells with atomic absorption analysis of pooled cell populations. We determine the magnesium peak-to-local continuum X-ray intensity ratio by electron probe X-ray microanalysis and calculate a mean cell magnesium concentration of 39 +- 19 mmol/kg dry weight from analysis of 100 cells. We determine a mean cell magnesium concentration of 34 +- 4 mmol/kg dry weight by atomic absorption analysis of pooled cells in three cell cultures. The mean cell magnesium concentrations determined by the two methods are not significantly different. We find a 10% coefficient of variation for both methods of ...
An x-ray fluorescence spectrometer was designed and fabricated which nondestructively determines the thickness of aluminum cladding at small suspected thin spots in the inner or outer surface of actinide reactor tubes. The analysis method is based on the difference in absorption of actinide L/sub #alpha#/ and L/sub #beta#/ fluorescent x-rays in passing through the cladding. Calibration plots of the logarithm of the L/sub #beta#//L/sub #alpha#/ x-ray intensity ratio versus cladding thickness are linear to at least 40 mils for U-Al, U_3O_8-Al, and PuO_2-Al substrates. Accuracy and precision of the experimentally determined cladding thickness and evaluated for both uranium and plutonium substrates. Experimental thickness data are reported for 618 quality assurance analyses on six Mark 41 PuO_2-Al target tubes. An x-ray fluorescence cladding thickness monitor operated with a ...
The devised radionuclide analyzer for the determination of total sulfur in coal includes two radionuclide sources with different energies, which are accommodated in collimators fitted with adjustable diaphramgs. The sample compartment is located between the two sources. Moreover, an X-ray fluorescence standard can be slid into the sample compartment. A proportional detector for X-ray fluorescence and scattered gamma radiation is located off the sample compartment. The input of the proportional detector is interfaced to the output of a high-voltage supply, the output, to the information input of a control-and-evaluation unit. One of the control outputs of the control-and-evaluation unit is connected to the input of the sliding mechanism for the X-ray fluorescence standard. This arrangement enables automatic energy calibration of the analyzer. The analyzer can measure not only total sulfur in coal by radionuclide ...
Secondary ion mass spectrometry (SIMS), secondary electron microscopy (SEM) and X-rayanalysis have been applied to the measurement of U-bearing particles with the intent of gleaning information concerning their history and/or origin. The lead isotopic abundances are definitive indicators that U-bearing particles have come from an ore-body, even if they have undergone chemical processing. SEM images and X-rayanalysis can add further information to the study that may allude to the extent of chemical processing. The presence of 'common' lead that does not exhibit a radiogenic signature is clear evidence of anthropogenic origin. (author)
The present work gives preliminary results of analysis of drug mixtures (NEPHROSAL tea bag) and its water infusion. In a sample of dried drugs the elements K, Ca, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Pb were identified, whereas in their water infusion only Ca, Mn, Zn and Sr were found. The method applied was radionuclide X-ray fluorescence analysis using a radionuclide source "1"0"9Cd, a Si/Li semiconductor detector and a multichannel analyzer Canberra 8100. (author) 6 refs.; 3 figs.
A theoretical analysis is presented for the method of determining the concentration distribution of admixtures in zone melting and in the study of diffusion in melts. Continuous mode X-ray fluorescence analysis is considered. The convolution integral interpreting the analog output of the ratemeter was solved applying the mathematical apparatus of Z transformation. The feasibility of the method is tested on an example of the determination of tin distribution in tungsten. With respect to the statistical error (#delta#<1.5%), the maximum integration constant (100 s) and a very slow sample feed (0.025 mm/s) were used. The calculated transfer function reflects the total transfer function of the ratemeter and the recorder used. (M.D.).
In the framework of the search for a ceramic material usable in the radioactive waste storage, uranium and thorium phosphates have been investigated. Their experimental synthesis conditions have been entirely reviewed, they lead to the preparation of four new compounds: U(UO{sub 2})(PO{sub 4}){sub 2}, U{sub 2}O(PO{sub 4}){sub 2}, UCIPO{sub 4}, 4H{sub 2}O, and Th{sub 4}(PO{sub 4}){sub 4}P{sub 2}O{sub 7}. Experimental evidenced are advanced for non existent compounds such as: U{sub 3}(PO{sub 4}){sub 4}, U{sub 2}O{sub 3}P{sub 2}O{sub 7} and Th{sub 3} (PO{sub 4}){sub 4}. Characterization by several techniques (X-rays and neutron powder diffractions, UV-Visible and Infra-red spectroscopies, XPS,...) were performed. The ab initio structure determination of U(UO{sub 2})(PO{sub 4}){sub 2} has been achieved by X-rays and refined by neutron diffractions. Through its physico-chemical analysis, ...
In order to understand the resistance of passive films formed during corrosion processes, an analytical technique using x-raydiffraction was developed to examine the structure of metal in closest proximity to the metal/liquid interface. The in-situ structure at the metal liquid interface was examined for 90 % copper and 10 % nickel (90-10 Cu-Ni) in KOH solution at room temperature and at four different potentistatically controlled potentials ({minus}0.5 V, {minus}0.1 V, +0.5 V and +0.10 V versus Ni/NiO). The chemical changes at the metal interface were studied over a period of 48 hours. It was found that the integrity of the 90-10 Cu-Ni foil in KOH was lost after a continued application of the potential over 48 hours. The x-raydiffraction results indicated that the structure of both the inner and the outer passive layers, at {minus}0.5V and {minus}0.1 V (versus Ni/NiO), is comprised of Ni(OH){sub 2}, ...
X-raydiffraction was used to monitor the {ital in} {ital situ} reaction of Pd deposited on Si(111) at room temperature. An ordered silicide forms spontaneously beneath a poorly ordered overlayer. It is commensurate and strained at low coverage, but relaxes to an unstrained state above a critical thickness of 18 A. During both phases of growth sustained intensity oscillations are seen that correspond to a layerwise consumption of the substrate at the buried interface.
Nano-sized particles of a lithium ion conductive solid electrolyte, LiTi{sub 2}(PO{sub 4}){sub 3}, were prepared by laser ablation. The obtained particles were ca. 10nm in diameter. X-ray powder diffraction and Raman spectroscopy showed that they were amorphous with local structure similar to the crystalline counterpart. They were crystallized by the heating at ca. 630{sup o}C. (author)
The radial distribution function (RDF) derived from wide angle X-raydiffraction patterns gives additional information about the spatial distribution of atoms. Their radial distances and relative average coordination numbers can be calculated using appropriate mathematical procedures. 7 refs.
α-Galactosidases from thermophilic organisms have gained interest owing to their applications in the sugar industry. The α-galactosidases AgaA, AgaB and AgaA A355E mutant from Geobacillus...Full Text Available
DEXD/H-box RNA helicases couple ATP hydrolysis to RNA remodeling by an unknown mechanism. We used x-ray crystallography and biochemical analysis of the human DEXD/H-box...Full Text Available
The localization of gold in the synovial membrane of rheumatoid arthritis patients treated with sodium aurothiomalate was examined and quantitative analysis of epon-embedded sections was carried out...Full Text Available
The applicability of two nuclear analytical methods: radionuclide X-ray fluorescence analysis and radiometric titrations based on precipitate formations was studied in order to determine the heptacaine hydrochloride in solutions. The applied methods were evaluated based on the obtained sensitivity values.
The applicability of two nuclear analytical methods: radionuclide X-ray fluorescence analysis and radiometric titrations based on precipitate formations was studied in order to determine the heptacaine hydrochloride in solutions. The applied methods were evaluated based on the obtained sensitivity values. (author).
Enolase is a multifunctional enzyme that plays important roles in many biological and disease processes. α-Enolase from human liver (hENO1) was expressed as a soluble protein and purified by...Full Text Available
The three-dimensional structure of the human adenovirus-2 proteinase complexed with its 11 amino acid cofactor, pVIc, was determined at 2.6 A resolution by X-ray crystallographic analysis. The fold...Full Text Available
X-ray fluorescence analysis was used to determine the zinc content of the ''Perilacin'' powder and the ZnO content of the ''Epiderman-pix'' powder. The characteristic Ksub(#alpha#) line of zinc was excited using a "1"4"7Pm/Mo source (10"7 s"-"1) and the molybdenum Ksub(#alpha#) line (17.47 keV). 4 to 5% Zn and 45 to 49% ZnO were determined with a NaI(Tl) scintillation detector. The radiation intensity was found to decrease with particle size. (M.K.).
Radionuclide X-ray fluorescence analysis (XFA) was used in the determination of the contents of metal residues in dosing plates for coin minting. XFA was also used for the determination of the strontium/calcium ratio in bone samples of different animals with the aim to obtain information on the food composition of these animals. It was found that bones of different animals can be distinguished based on the Sr/Ca ratio. No significant differences in the Sr/Ca ratio were observed in human bones of individuals from different social groups. (author). 1 fig., 5 tabs., 4 refs.
Double-crystal high-resolution x-ray fluorescence spectrometry was applied to the state analysis of sulfur in coal and related fly ash. For total sulfur, a proportional relationship exists between fluorescence intensities and the analytical values obtained by the oxygen-combustion method. Two oxidation states of sulfur were identified by a least square curve fitting method, by assuming that the spectrum profile is identical for each sulfur state but the intensity and position are different. The chemical state of sulfur in coal and remaining in fly ash is discussed.
The paper presents an integrated approach to the problem of electron temperature diagnostics of the plasma in a reversed field pinch. Three different methods, sampling different portions of the electron distribution function, are adopted, namely Thomson scattering, soft X-ray spectroscopy by pulse-height analysis and filtered soft X-ray intensity ratio. A careful analysis of the different sources of systematic errors is performed and a novel statistical approach is adopted to mutually validate the three independent measurements. A satisfactory agreement is obtained over a large range of experimental conditions, indicating that in the plasma core the energy distribution function is well represented by a maxwellian. (author)
The usefulness and clinical applicability of computed radiography(FCR) in X-ray examination of the stomach were evaluated in comparison with film-screen (FS) radiography by both phantom experiments and clinical studies. Receiver operating characteristic (ROC) curve analysis consisting of 25 normal and 25 artificially created simulated lesions on an orginally created Styrofoam phantom showed no difference in lesion detectability between FCR and FS radiography. Both were also equal in evaluation of the internal structure and margin of the 25 lesions by visual ranking. ROC curve analysis of clinical cases was performed in 30 cases, 20 normal and 10 abnormal, while evaluation by visual ranking was performed on 18 lesions. There was no significant difference between FCR and FS radiography either with ROC curve analysis or visual ranking, although the variations were somewhat greater in the clinical cases ...
The usefulness and clinical applicability of computed radiography(FCR) in X-ray examination of the stomach were evaluated in comparison with film-screen (FS) radiography by both phantom experiments and clinical studies. Receiver operating characteristic (ROC) curve analysis consisting of 25 normal and 25 artificially created simulated lesions on an orginally created Styrofoam phantom showed no difference in lesion detectability between FCR and FS radiography. Both were also equal in evaluation of the internal structure and margin of the 25 lesions by visual ranking. ROC curve analysis of clinical cases was performed in 30 cases, 20 normal and 10 abnormal, while evaluation by visual ranking was performed on 18 lesions. There was no significant difference between FCR and FS radiography either with ROC curve analysis or visual ranking, although the variations were somewhat greater in the clinical cases ...
The emission of the plerion G21.5-0.9 appears more extended in Xrays than in radio. This is an unexpected result because it would imply that short-lived X-ray electrons may reach distances even larger than radio electrons. Applying an empirical relationship between dust scattering optical depth and photoelectric column density, the measured column density leads to a large optical depth at 1 keV, of about 1. Therefore we investigate the hypothesis that the detected halo be an effect of dust scattering, re-analyzing an Cal/PV XMM-Newton observation of G21.5-0.9 and critically examining it in terms of a dust scattering model. We also present a spectral analysis of a prominent extended feature in the northern sector of the halo.
The present paper is a comparative study of the cerium-containing nickel catalysts supported on x- and y-zeolites. In general, the addition of cerium ions caused an increase in the catalytic activity for CO hydrogenation and shifted the product selectivity to high molecular weight hydrocarbons. The degree of the effect of cerium additive depends on the ratio of cerium to nickel contents, the reduction temperature, and the nature of the supporting materials. Catalyst characterization, including volumetric hydrogen chemisorption, temperature programmed reduction/desorption, x-raydiffraction, surface area measurements, in-situ infrared spectroscopy and x-ray photoelectron spectroscopy, was performed in order to interpret the phenomena due to the effects of cerium additives and the support effect on Ni/zeolite catalysts.
Self-amplifying spontaneous radiation free-electron lasers, such as the LCLS or the European X-FEL, rely on the incoherent, spontaneous radiation as the seed for the amplifying process. Though this method overcomes the need for an external seed source one drawback is the incoherence of the effective seed signal. The FEL process allows for a natural growth of the coherence because the radiation phase information is spread out within the bunch due to slippage and diffraction of the radiation field. However, at short wavelengths this spreading is not sufficient to achieve complete coherence. In this presentation we report on the results of numerical simulations of the LCLS X-ray FEL. From the obtained radiation field distribution the coherence properties are extracted to help to characterize the FEL as a light source.
The local strain and texture in Al interconnect wires have been investigated using white and monochromatic x-ray microbeams on the MHATTCAT undulator beam line at the Advanced Photon Source. Intergrain and intragrain orientations were obtained with ~0.01 degree sensitivity using white beam measurements on wide Al pads (~100 Mu-m) and thin (2 Mu-m) Al wires. Orientation changes of up to 1 degree were found within individual grains of the (111) textured Al interconnects. Deviatoric strain measurements indicate small intragranular strain variations, but intergranular strain variations were found to be quite large.
Metal-organic chemical vapor deposition (MOCVD) made layers of strontium-bismuth-tantalate (SBT) were characterized by spectroscopic ellipsometry (SE) using the Adachi model [S. Adachi, Phys. Rev. B 35 (1987) 7454-7463]. The evaluated optical parameters were correlated with the physical and chemical behavior examined by X-raydiffraction (XRD). As a result, it was possible to fit the measured spectra with the Adachi model in a wide range covering the region of the band gap. The Adachi model provides electronic layer parameters like the transition energy E 0 and broadening ?. Our investigations established a correlation between XRD-determined average grain size and the electronic layer parameters.
X-Ray reflectivity has been used to investigate the microstructural changes of solution-cast stearic acid films before and after immersion in CoCl{sub 2} solutions. Before immersion, the films possess a well-defined layered structure with an interlayer spacing of 4.01{+-}0.05 nm. After the films were immersed in the CoCl{sub 2} solutions, a new set of equidistant diffraction peaks emerge, the corresponding interlayer spacing of which is 5.13{+-}0.05 nm. The X-ray photoelectron spectra of the films indicate the existence of cobalt ions inside the films after immersion. It is concluded that the permeation of the cobalt ions into the hydrophilic interlayer causes the stearic acid molecules to reorient perpendicular to the films, resulting in the increase of interlayer spacing and the roughening of the interfaces.
In order to reduce the activation temperature of the TiZrV alloy, thin films of various compositions were produced by three-cathode magnetron sputtering on stainless-steel substrates. For the characterisation of the activation behaviour the surface chemical composition has been monitored by Auger electron spectroscopy during specific in situ thermal cycles. The volume elemental composition of the film has been measured by energy dispersive X-ray spectroscopy and the morphology (crystal structure and size of the crystallites) has been investigated by X-raydiffraction. The criteria indicating the sample quality and its dependence on film structure and chemical composition are presented and discussed. (13 refs).
Accelerated aging tests on gold bridgewired detonator assemblies to determine compatibility of the Au and Pd-In-Sn solder with the organic explosive, PENT, have revealed an unusual corrosion process. These tests, conducted at 74/sup 0/C and 54/sup 0/C indicated a preferential attack of the gold. A matrix of corrosion test units was established to study this corrosion problem with accelerating temperatures up to 100/sup 0/C. Scanning electron microscopy (SEM), energy dispersive x-ray (EDX), and x-raydiffraction techniques were used to determine the extent of the corrosion and identify the corrosion products. Results indicate the preferential attack of the gold was due to HCN formed by decomposition of the explosive powder (PETN) at high temperatures. Other associated reactions were also observed including subsequent attack of the solder by the gold corrosion product and degradation of the plastic header.
SBA-15 supported nano-scaled copper oxide was synthesized by impregnation method via ultrasonic-assisted route. The removal test from gas mixture containing 0.1?vol.% hydrogen sulfide was carried out over this material at atmospheric conditions. The effects of the chemical nature of copper oxide and the textural properties of the material on removal capacity were studied. The materials before and after the removal test were analyzed by nitrogen adsorption, X-raydiffraction, Transmission Electron Microscope, X-ray photoelectron Spectroscopy, Fourier Transform Infrared Spectrometer and Inductive Coupled Plasma. The results showed that copper species are located predominantly in mesopore channels, existing as copper oxide nanoparticles. Mesopores are active sites for removal reaction. The ou...
Full text: Institute for Nuclear Research, Pitesti-Mioveni, Romania in direct cooperation with the National Institute for Laser, Plasma and Radiation Physics, Magurele, Bucharest studied and prepared for coating more than 1000 tiles made of Inconel with 7-9 #mu#m of beryllium for nuclear fusion applications at JET, Culham, UK. The principles of manufacturing processes using thermal evaporation and plasma ignited in pure metal vapors as well as by Thermionic Vacuum Arc (TVA) method and the properties of the Ni and Be coatings are presented. The prepared beryllium layers were characterized by scanning electron microscopy, transmission electron microscopy, X-raydiffraction, X-ray photoelectron spectroscopy and atomic force microscopy. (authors)
A novel single-step synthetic method for the preparation of anatase N-doped TiO"2 nanocrystalline at low temperature has been devoleped. The N-doped anatase TiO"2 nanoparticles were synthesized by sonication of the solution of tetraisopropyl titanium and urea in water and isopropyl alcohol at 80^oC for 150min. The as-prepared sample was characterized by X-raydiffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and UV-vis absorption spectrum. The product structure depends on the reaction temperature and reaction time. The photocatalytic activity of the as-prepared photocatalyst was evaluated via the photodegradation of an azo dye direct sky blue 5B. The results show that the N-doped TiO"2 nanocrystalline prepared via sonication exhibit an excellent photocatalytic...
We describe a camera to record coherent scattering patterns with a soft-x-ray free-electron laser (FEL). The camera consists of a laterally graded multilayer mirror, which reflects the diffraction pattern onto a CCD detector. The mirror acts as a bandpass filter for both the wavelength and the angle, which isolates the desired scattering pattern from nonsample scattering or incoherent emission from the sample. The mirror also solves the particular problem of the extreme intensity of the FEL pulses, which are focused to greater than 10"1"4 W/cm"2. The strong undiffracted pulse passes through a hole in the mirror and propagates onto a beam dump at a distance behind the instrument rather than interacting with a beam stop placed near the CCD. The camera concept is extendable for the full range of the fundamental wavelength of the free electron laser in Hamburg (FLASH) FEL (i.e., between 6 and 60 nm) and into the water window. We have fabricated and ...
The effect that different chemical and physical atomic environments can have on the relative intensities of radiative electron transitions from the filling of K shell vacancies was investigated. The method used involved the detection of photoionization induced X-ray fluorescence. An experimental system based on a hyper pure germanium detector (HPGE) was used to measure the relative K-L and K-M X-ray yields from the photofluorescence of a series of lanthanide elements and compounds. A background subtraction and peak integration strategy was employed which accounted for scattering in the samples and scattering of the flux from the radioisotope photoionization sources. Analysis of the data resulted in a tabulation of relative K/sub ..beta..//K/sub ..cap alpha../ X-ray intensity ratios. The measured relative K/sub ..beta..//K/sub ..cap alpha../ X-ray intensity ratios were compared to ...
The effect that different chemical and physical atomic environments can have on the relative intensities of radiative electron transitions from the filling of K shell vacancies was investigated. The method used involved the detection of photoionization induced X-ray fluorescence. An experimental system based on a hyper pure germanium detector (HPGE) was used to measure the relative K-L and K-M X-ray yields from the photofluorescence of a series of lanthanide elements and compounds. A background subtraction and peak integration strategy was employed which accounted for scattering in the samples and scattering of the flux from the radioisotope photoionization sources. Analysis of the data resulted in a tabulation of relative K/sub #beta#//K/sub #alpha#/ X-ray intensity ratios. The measured relative K/sub #beta#//K/sub #alpha#/ X-ray intensity ratios were compared to the calculated ...
Exploration for epithermal Au has been active lately in the Aegean Sea of the eastern Mediterranean Basin, both in the islands of the Quaternary arc and in those of the back-arc region. The purpose of this study was the structural mapping and analysis for a preliminary investigation of possible epithermal gold mineralization, using remotely sensed data and techniques, structural and field data, and geochemical information, for a specific area on the Island of Lesvos. Therefore, Landsat-TM and SPOT-Pan satellite images and the Digital Elevation Model (DEM) of the study area were processed digitally using spatial filtering techniques for the enhancement and recognition of the geologically significant lineaments, as well as algebraic operations with band ratios and Principal Component Analysis (PCA), for the identification of alteration zones. Statistical rose diagrams and a SCHMIDT projection Stereo Net were generated from the lineament maps and ...
With recent and archival Rossi X-Ray Timing Explorer (RXTE) X-ray measurements of the heavily obscured X-ray pulsar EXO 1722-363 (IGR J17252-3616), we carried out a pulse timing analysis to determine the orbital solution for the first time. The binary system is characterized by a_x sin(i) = 101 +/- 3 lt-s and P_orb = 9.7403 +/- 0.0004 days (90% confidence), with the precision of the orbital period being obtained by connecting datasets separated by more than 7 years (272 orbital cycles). The orbit is consistent with circular, and e 61 degrees at the 99% confidence level, the radius of the primary is between 21 R_sun and 37 R_sun, and its mass is less than about 22 M_sun. The acceptable range of radius and mass shows that the primary is probably a supergiant of spectral type B0I-B5I. Photometric measurements of its likely counterpart are consistent with the spectral type and luminosity if the distance to ...
Silver iron oxide nanoparticles of fairly small size (average diameter approximately 1 nm) with narrow size distribution have been synthesized by the interaction of colloidal beta- Fe2O3 and silver nanoparticles. The surface morphology and size of these particles have been analyzed by using atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Their structural analysis has been carried out by employing x-raydiffraction (XRD), selected-area electron diffraction (SAED), optical and infrared (IR) spectroscopic techniques. The ageing of these particles exhibits the formation of self-assembly, possibly involving weak supramolecular interactions between Ag(I)O4 and Fe(III)O4 species. These particles display the onset of absorption in the near-infrared region and have higher absorption coefficient in the visible range compared to that of ...
The development of the microstructure on aging of an (#alpha# + #beta#) type titanium alloy containing 6Al-1.6Zr-3.3Mo-0.3Si (VT9) (in weight percent) has been studied. The #beta#-transus temperature of this alloy is approximately 1243 K. Solution treatment in the #beta#-phase field of the alloy followed by quenching in water at room temperature resulted in the formation of a single-phase martensite structure. The martensitic structure was confirmed to be orthorhombic (#alpha# double-prime) using X-raydiffraction. The water-quenched (WQ) specimens were subjected to aging treatments at temperatures of 823, 873, and 973 K for various lengths of time. Aging at 823 K for times between 24 and 100 hours did not bring about any noticeable change in the microstructure. Aging at 823 K for 200 and 300 hours resulted in the heterogeneous precipitation of s_2 silicide particles and thin films of #beta# sandwiched between the interplatelet boundaries of ...
This work reports studies of ethanol oxidation on Pt-Sn/C catalysts with nearly the same particle size and identical overall composition having different amounts of oxide and alloyed phases. Results of characterization of physical properties by transmission electron microscopy (TEM), X-raydiffraction (XRD), differential scanning calorimetry (DSC), X-ray photoelectron spectroscopy (XPS), and in situ dispersive X-ray absorption spectroscopy (DXAS) are presented. The variation in the amount of oxide and alloyed phases, promoted by heat treatments in mild temperature conditions, does not produce any significant particle growth. Cyclic voltammetry and oxidation of adsorbed CO in acid medium are used to probe the surface conditions. Data on the electrocatalytic activity towards ethanol oxidation, obtained by potential sweeps and chronoamperometry, are discussed and correlate well with the physical ...
Based on the instrumental wavelength dispersive X-ray fluorescence technique of analysis (W D-X R F), the inorganic elements in four samples of commercial medicines drugs were analyzed. The samples were used without any chemical separation of the elements or chemical pre-treatment. Eleven elements could be identified, namely Si, P, S, Cl, K, Ca, Ti, Mn, Fe, Cu and Zn. However, Si, Ti and Mn have not been mentioned in the printed instructions for the use of the medicines drugs by the producers. (author)
The study of imported ceramics found in Beirut and suspected to belong to north Syrian products will provide key evidence for the roles in trade of the various postulated centers in northern Syria and northern Lebanon. It is proposed that a comprehensive range of likely north Syrian products imported to Beirut will be chemically analyzed by PIXE (proton induced X-ray emission) in order to characterize, compare and isolate the various regional production centers that supplied the city from the Persian to Byzantine periods. In this work, we were mainly focusing on the characterization of Amrit products, by using 3 MeV proton beam and Al funny filter, as X-ray absorber.
Radionuclide X-ray fluorescence method with a Si/Li semiconductor detector and "2"3"8Pu exciting source was used in the study of Mn, Fe, Cu, Zn, and Pb content of solid emissions, raw and final materials of a brick factory. From the point of view of metal content, the working environment if the brick factory is safe for workers. (author) 2 refs.; 2 figs.; 1 tab.
In an effort to explore Diffraction Enhanced Imaging of bone tissue, experiments were performed to determine if it was possible to use Diffraction Enhanced Imaging to detect microdamage in bovine cortical bone. Measurements were made at the National Synchrotron Light Source where pre- and post-fatigue rocking curve widths of the bone were studied. The rocking curve widths were then compared. Since no consistent pattern of narrowing or broadening of the rocking curve emerged, it is likely that the ultra-small-angle X-ray scattering present in the bone overshadowed any additional changes to rocking curve caused by microdamage of the bone. Larger bone structures were able to be visualized which suggests that microdamage may be visualized with a higher resolution detector.
The energy dispersive beamline X6A at the National Synchrotron Light Source employs a curved crystal monochromator (polychromator) which focuses a range ([similar to]1 keV) of x-ray energies into a narrow (100--120 [mu]m) line image. Although this beamline was constructed primarily for time-dependent EXAFS experiments, we have begun to explore the use of this instrument for energy dispersive diffraction experiments with different types of sample including macromolecular crystals. The tunability ([ital E]=6.5 to 21 keV) and flexibility ([Delta][ital E]=100--1000 eV) of the instrument makes the beamline ideal as a test bed for the application of polychromatic single-crystal diffraction techniques to different chemical or biological materials.
Focused ion beam (FIB) microscopes have become well-established in the semiconductor industry during the past decade, and are rapidly gaining attention in the field of materials science, both as a tool for producing site specific, parallel sided transmission electron microscope (TEM) specimens and as stand alone specimen preparation and imaging systems. FIB secondary electron imaging (SEI) of nickel-based alloys, such as commercially produced Alloy 600 (approximately Ni 15Cr 10Fe 0.5C), has been demonstrated to show a high degree of sensitivity to the presence of deformation in the alloy, and FIB secondary ion imaging (SII) is particularly useful for identifying the presence of grain boundary corrosion, as secondary ion yields from metallic specimens can increase by three orders of magnitude in the presence of oxygen. This 'oxygen enhanced yield', makes FIB SII ideal for detection of corrosion at grain boundaries down to thicknesses of only a few tens of nanometers. Historically, while ...
Available in abstract form only. Full text of publication follows: The application spectrum of X-ray and Gamma radiation is increasing exponentially in the area of diagnostic, nuclear medicine, food preservation, nuclear power plants and strategic utilities. To prevent the harmful effects of these radiations, shielding materials based on lead metal and its compounds are being used historically, which are toxic in nature. To protect environment it has become necessary to develop non-toxic lead free shielding materials. The use of titanium metal and its compounds as synthetic rock i.e. SYNROC are reported to be very effective non-toxic shielding materials for various applications. Red mud waste generated in aluminum producing industries possesses a unique mineralogical compositions containing fairly high quantity of titanium oxide and iron oxide useful for making non toxic shielding compositions and therefore red mud has been utilized for the first time in the world ...
Kbeta-to-Kalpha X-ray intensity ratios of Ti and Ni have been measured in pure metals and in alloys of Ti(x)Ni(1-x) (x=0.7, 0.6, 0.5, 0.4 and 0.3) following excitation by 22.69 keV X-rays from a 10 mCi (109)Cd radioactive point source. The valence-electron configurations of these metals were determined by corporation of measured Kbeta-to-Kalpha X-ray intensity ratios with the results of multiconfiguration Dirac-Fock calculation for various valence-electron configurations. Valence-electron configurations of 3d-transition metals in alloys indicate significant differences with respect to the pure metals. Our analysis indicates that these differences arise from delocalization and/or charge transfer phenomena in alloys. Namely, the observed change of the valence-electron configurations of metals in alloys can be explained with the transfer of 3d electrons from one element to the other element and/or the ...
K?-to-K? X-ray intensity ratios of Ti and Ni have been measured in pure metals and in alloys of TixNi1-x (x=0.7, 0.6, 0.5, 0.4 and 0.3) following excitation by 22.69 keV X-rays from a 10 mCi 109Cd radioactive point source. The valence-electron configurations of these metals were determined by corporation of measured K?-to-K? X-ray intensity ratios with the results of multiconfiguration Dirac-Fock calculation for various valence-electron configurations. Valence-electron configurations of 3d-transition metals in alloys indicate significant differences with respect to the pure metals. Our analysis indicates that these differences arise from delocalization and/or charge transfer phenomena in alloys. Namely, the observed change of the valence-electron configurations of metals in alloys can be explained with the transfer of 3d electrons from one element to the other element and/or the rearrangement of ...
In this work a comprehensive metallophysical study was carried out for two aluminosilicide slip coatings of the systems Al-Si and Al-Nb-Si and an electron-beam Co-Cr-Al-Y coating on alloy EP-539 (17...19% Cr, 4...6% Co, 2.5...4% W, 4.5...6.5% Mo, 2...3% Ti, 3...4% Al, 1.4...2% Nb, balance Ni) after high-temperature testing. The protective properties of the coatings were evaluated from the results of laboratory tests for heat resistance at 1000/sup 0/C in the combustion products of diesel fuel with added sulfur at 970, 1000, and 1060/sup 0/C for 100 h and after full-scale tests for 150, 250, 400, and 700 h. Metallographic, hardness, x-ray, and micro x-ray studies of the coating were carried out. Layer-by-layer phase composition and the lattice spacing of the main phases were determined. X-rayanalysis was carried out in an a DRON-1 diffractometer in copper K/sub ..-->../-radiation, and ...
We studied the strain introduced in a Si(111) substrate due to MeV ion implantation using extremely asymmetric x-raydiffraction and measured the rocking curves of asymmetrical 113 diffraction for the Si substrates implanted with a 1.5 MeV Au"2"+ ion at fluence values of 1x10"1"3, 5x10"1"3, and 1x10"1"4/cm"2. The measured curves consisted of a bulk peak and accompanying subpeak with an interference fringe. The positional relationship of the bulk peak to the subpeak and the intensity variation of those peaks with respect to the wavelengths of the xrays indicated that crystal lattices near the surface were strained; the lattice spacing of surface normal (111) planes near the surface was larger than that of the bulk. Detailed strain profiles along the depth direction were successfully estimated using a curve-fitting method based on Darwin's dynamical diffraction ...
The handling of physical-nuclear techniques for the analysis of archaeological pieces it was carried out by first time in 1956 by the doctors Oppenheimer and Dodsom (in the United States); who wrote about the wide utilities of the neutron activation analysis (NAA), this technique requires of a nuclear reactor that could be considered like one a factory of thermal neutrons necessary to carry out this analysis. The first experiments in that were applied the NAA were on ceramic coming from the Mediterranean, in those that the relationships of the elements of sodium and manganese were determined to know their elementary composition and to identify the origin of their manufacture. Later on other study techniques were applied in archaeological materials, as the X-ray fluorescence, Moessbauer spectroscopy, scanning electron microscopy, PIXE analysis (particle induced ...
The thermal stability of low-friction Me-C/a-C:H coatings is important for their potential applications in the tool and automotive industry. Recently we showed that CrC _x/a-C:H coatings prepared by unbalanced magnetron sputtering of a Cr target in Ar + CH_4 glow discharges exhibit a nanocomposite structure where metastable fcc CrC nanocrystals are encapsulated by an a-C:H phase. Here, we present the structural evolution of these nanocomposite CrC/a-C:H coatings during annealing. High-temperature X-raydiffraction in vacuum and differential scanning calorimetry (DSC) combined with thermo-gravimetric analysis in Ar atmosphere indicate decomposition of the formed metastable fcc CrC phase and subsequent formation of Cr_3C_2 and Cr_7C_3 and structural transformation of the a-C:H matrix phase towards higher sp"2 bonding contents at temperatures above 450 deg. C. Combined DSC and mass spectrometer analysis as ...
The in-situ measurement of a crystallographic texture is a special type of a non-destructive measurement, which need special equipments. Due to the high photon flux and the excellent brilliance high energetic synchrotron radiations are a fantastic tool particular in fast experimentation. Moreover, a high penetration power allows the investigation of standard tensile sample of the DIN-norm. A loading device with a power up to 20 kN was installed at the hard wiggler beamline BW5 (HASYLAB-DESY) to perform in-situ strain and in-situ texture analysis. Using 100keV X-rays one gets short wavelength so that a 2D image-plate detector offers a wide range of diffraction pattern within the first 10 degree in 2 theta. Thermal neutron is another radiation with a high penetration power, which is the standard method for global texture analysis of bulk samples. As an example rectangular extruded Mg- Az31 was ...
It has been discovered that the presence of MoO/sub 3/ lowers the ..cap alpha..-..beta.. transition in Sb/sub 2/O/sub 4/ from 935 to 850/sup 0/C with concurrent dissolution of Mo in the high-temperature (..beta..) form. The structure of Mo-doped ..beta..-Sb/sub 2/O/sub 4/ has been investigated by powder neutron diffraction, extended X-ray absorption fine structure (EXAFS) and Raman spectroscopies, and scanning-electron microscopy (SEM). Cell parameters: a = 12.0571 (12) A, b = 4.8335 (1) A, c = 5.3838 (6) A, ..beta.. = 105.579 (5)/sup 0/, monoclinic, space group C2/c, Z = 4. Combining the results of these techniques leads to the hypothesis that Mo is located interstitially within channels of electron density in the Sb/sub 2/O/sub 4/ structure with concurrent vacancy of two Sb/sup III/ atoms. There is no apparent oxygen deficiency in the resulting structure. 25 references, 6 figures, 3 tables.
Nanocomposites containing polyethylene (PE) and montmorillonite clay organically modified (OMMT) with quaternary ammonium salts were obtained via direct melt intercalation. A montmorillonite sample from the Brazilian state of Paraiba was treated with four different types of quaternary ammonium salts. After the treatment, the powder was characterized by X-raydiffraction and scanning electron microscopy. The dispersion and morphologies of OMMT within PE were investigated by X-raydiffraction and transmission electron microscopy. The results revealed the formation of intercalated montmorillonite layers in the PE matrix. The thermal stability and flammability of the PE/montmorillonite clay nanocomposites were measured by thermogravimetry and horizontal burning tests for HB classification, Underwrites Laboratories (UL 94), respectively. It was shown that the samples do not degrade at the processing ...
The influence of Cr on the structure and electrochemical properties of LiCoVO{sub 4} was studied using X-Raydiffraction, scanning electron microscopy, Raman Spectroscopy and cycle tests. Doping levels up to 10 mol% were achieved, which improved the electrochemical stability of the structure of LiCoVO{sub 4}, resulting in a significant increase in the initial charge and discharge capacity. The Raman spectroscopy data for the Cr-doped LiCoVO{sub 4} is similar as for LiCoVO{sub 4}. The replacement of a dopant for the Co-ion in the inverse spinel structure causes several Raman shifts. The X-raydiffraction patterns show no new phases and combined with the Raman spectroscopy data it is concluded that the Cr dopant will be located at the octahedral site (16d) where they create an electronic pathway that enhances the electronic conductivity. However, the capacity dropped significantly after prolonged cycling, ...
A knowledge of surface film growth kinetics can be quite useful in the production of materials for uses ranging from protective coatings to microelectronic devices. A technique for determining the kinetics of film growth is presented which should prove to be a valuable alternative to the array of spectroscopies (AES, RBS, etc.) currently favored for these measurements. Some of the virtues of this X-raydiffraction approach are its non-destructive nature, thickness resolution better than 50 {angstrom} and conventional equipment requirements. Results obtained for the growth of Pd{sub 2}Si films during thermal annealing of Pd coatings on Si, indicate parabolic growth over a temperature range of 160-222 C. The rate constant was found to be k{prime} = 7 {times} 10{sup {minus}4} exp ({minus}1.06 eV/kT) cm{sup 2}/sec, where (film thickness){sup 2} = k{prime} x time. This activation energy is in agreement with results obtained by other techniques. A ...
Three types of titanium hydrides have been reported: #delta#, #epsilon# and #gamma# hydrides. The #delta# hydride forms in the composition range from TiH/sub 1.5/ to TiH/sub 1.99/ and has a CaF/sub 2/ structure with metal atoms on an fcc lattice and hydrogen atoms randomly occupying tetrahedral interstitial sites. At higher hydrogen concentrations, TiH/sub 2/, the fct (c/a # #epsilon# transformation is apparently diffusionless, similar to that operating in the cubic/tetragonal transformation in zirconium hydride. The metastable fct #gamma# hydride having a c/a value of 1.09 or 1.12 forms from solid solutions of hydrogen in the hcp #alpha# matrix. While the titanium hydride precipitation in #alpha#-Ti and its alloys has attracted extensive investigation, hydride formation in bcc #beta#-Ti alloys has rarely been studied because they have not been thought to be liable to hydride formation. This paper shows conclusive evidence for the fcc #delta# hydride phase formation in the #beta# phase ...
X-ray magnetic diffraction (XMD) technique was applied to an orbital ordering compound of ferromagnetic YTiO_3 for the first time. The orbital-magnetic form factor #mu# _L(k) and the spin-magnetic form factor #mu# _S(k) were independently measured by utilizing the LS separation ability of the XMD. The #mu# _L(k) was measured for ten reciprocal-lattice points. No significant values of the #mu# _L(k) were observed for most of the reciprocal-lattice points within the estimated statistical errors, which suggested quenching of the orbital moment. The #mu# _S(k) was measured for 22 reciprocal-lattice points. Fourier synthesis of the #mu# _S(k) gave the spin density distribution m _S(r) in the real space. The obtained m _S(r) map shows the characteristic feature of the electron distribution of 3d electron in the t_2_g state of a Ti atom coordinated by O"2"- ions, in which the electrons are distributed away from the negative O"2"- ions. It is concluded ...
Crystalline bis(O,O'-di-sec-butyldithiophosphato)platinum(II) was prepared and studied by means of 13C, 31P CP/MAS NMR spectroscopy and single-crystal X-raydiffraction. The unit cell of the platinum(II) compound is comprised of one centrosymmetric mononuclear molecule [Pt{S2P(O-sec-C4H9)2}2], in which the dithiophosphate groups display structural equivalence in both 31P NMR and XRD data. A pair of the dithiophosphate ligands exhibit the same S,S'-bidentate chelating structural function and form two planar four-membered chelate rings, [PtS2P], in this molecule. The planar configuration of the [PtS4] chromophore in structure 1 is governed by the dsp2-hybrid state of platinum(II). The structural states of the dithiophosphate groups in two different samples of complex 1 (one crystallised from...
Liquid high-level nuclear waste will be immobilized at the Savannah River Site (SRS) by vitrification in borosilicate glass. The glass will be produced and poured into stainless steel canisters in the Defense Waste Processing Facility (DWPF). Eventually these canistered waste forms will be sent to a geologic repository for final disposal. In order to assure acceptability by the repository, the Department of Energy has defined requirements which DWPF canistered waste forms must meet. These requirements are the Waste Acceptance Preliminary Specifications (WAPS). The WAPS require DWPF to identify the crystalline phases expected to be present in the final glass product. Knowledge of the thermal history of the borosilicate glass during filling and cooldown of the canister is necessary to determine the amount and type of crystalline phases present in the final glass product. Glass samples of seven projected DWPF compositions were cooled following the same temperature profile as that of glass ...
Three typical Japanese coals of non-coking coal, coking coal and anthracite were heat-treated with KOH, and change in their pore structure was examined by absorption of N2, X-raydiffraction and TEM observation. In addition, the relation between a coal rank and pore structure was also studied by absorption experiment of N2. In experiment, the mixture of coal and KOH in a nickel holder was heat-treated in N2 gas flow at heating rate of 2{degree}C/min, and held at a fixed temperature for one hour. To clarify the pore structure, N2 absorption isotherms were measured at -196{degree}C under nearly 76cmHg using a commercially available full-automatic absorption measurement equipment. Based on the X-raydiffraction and TEM observation results on activated coals, the relation between the N2 absorption and pore structure was studied. The results are summarized as follows: (1) The yield and absorption ability of ...
Single-crystalline cadmium selenide nanoparticles were obtained using high-temperature solution phase synthesis (HTSPS) synthesis. X-Ray powder diffraction and transmission electron microscopy were used to confirm the crystallinity and morphology of the resulting nanoparticles. To study the action of CdSe on antioxidant activity, we selected two biotechnological important strains of microalgae: cyanobacteria Spirulina platensis and red microalgae Porphyridium cruentum. In the case of Porphyridium cruentum, the obtained results demonstrated an increase in the productivity. For Spirulina platensis, the presence of the compound in the cultivating medium decreased the productivity of cyanobacteria.
17-4PH stainless steel was modified by direct current (DC) plasma nitriding and titanium nitride film duplex treatment in this study. The microstructure, wear resistance and corrosion resistance were characterized by X-raydiffraction (XRD), pin-on-disk tribological test and polarization experiment. The results revealed that the DC plasma nitriding pretreatment was in favor of improving properties of titanium nitride film. The corrosion resistance and wear resistance of duplex treatment specimen was more superior to that of only coated titanium nitride film.
17-4PH stainless steel was modified by direct current (DC) plasma nitriding and titanium nitride film duplex treatment in this study. The microstructure, wear resistance and corrosion resistance were characterized by X-raydiffraction (XRD), pin-on-disk tribological test and polarization experiment. The results revealed that the DC plasma nitriding pretreatment was in favor of improving properties of titanium nitride film. The corrosion resistance and wear resistance of duplex treatment specimen was more superior to that of only coated titanium nitride film.
Methods of X-raydiffraction and transmission electron microscopy were used to study the microstructure of dispersion-strengthened Cu-Al2O3 nanocomposites obtained by the method of simultaneous deposition of Cu and Al2O3 from the vapor phase. The effect of the size of particles of the oxide (Al2O3) and of their content on the electrical resistance of the composite has been considered. The results obtained make it possible to suppose that the main structural factor that determines the electrical resistance of the composite are nanodispersed particles of Al2O3 with a size of less than 20 nm.
The mechanism of abrupt increase of the giant magneto impedance (GMI) ratio in the ion irradiated Co-based amorphous ribbon has been investigated. The grazing incident X-raydiffraction and transmission electron microscope were used to characterize the samples before and after ion irradiation. The GMI-ratio considerably increased in the ion irradiated samples and the GMI response showed strong dependence on the driving frequencies. The Barkhausen noise (BN) signals are increased for the Ar ion irradiated sample with dose of 1x10^1^7 ion/cm^2. The results are interpreted in terms of GMI variation associated with domain wall dynamics.
Metallic multilayers offer a fantastic playground to investigate elastic stresses in films of nanometer thickness. We will present and discuss a few examples from our recent work on Au-Ni and Ag-Cu systems where we combined plate bending measurements and electron or X-raydiffraction to investigate stress buildup and interfacial mixing. Comparing these two cases we discuss the results with respect to basic parameters like the misfits in lattice parameters and in elastic moduli, the mixing enthalpies and the surface energies.
HgTe rod-shape composed of crystalline particles has been prepared by a hydrothermal method, and characterized by means of X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transition electron microscopy (TEM). The effects of capping agents, reductants, reaction temperatures, and reaction times on crystal structures and shapes of HgTe have been investigated. The results showed that the CTAB as capping agent plays a crucial role in the hydrothermal process. The synthesis procedure is simple and uses less toxic reagents than the previously reported methods.
Depth resolved positron annihilation studies on Pd/Si thin film system have been carried out to investigate silicide phase formation and vacancy defect production induced by thermal annealing. The evolution of defect sensitive S-parameter clearly indicates the presence of divacancy defects across the interface, due to enhanced Si diffusion beyond 870 K consequent to silicide formation. Corroborative glancing incidence X-raydiffraction (GIXRD), Auger electron spectroscopy (AES) and Rutherford backscattering spectrometry (RBS) have elucidated the aspects related to silicide phase formation and Si surface segregation.
A study is reported of the use of three types of fly ash as a raw material in the production of a potassium silicate fertilizer. The results of high-temperature X-raydiffraction, calcination tests and chemical analyses indicate that a potassium silicate fertilizer conforming with fertilizer specifications can be produced by appropriate regulation of calcining temperature and the amounts of Fe/sub 2/0/sub 3/, Al/sub 2/O/sub 3/, MgO and CaO added. The results of tests of fertilizers incorporating red mud are also reported.
The low alloy steels were nitrided in the plasma atmosphere generated by using hollow cathode discharge. For comparison, specimens of 40 Cr steel were in two different potential states. One kind is isolated from cathode and anode between them the discharge was created. The other kind is placed on the plate which is connected to the cathode. The nitriding was carried out at different temperatures. The surface morphology, phase of compound layers and microhardness profiles were analyzed. The optical microscopy observation and X-raydiffraction showed that the compound layers were formed in all experiments. The results of the nitriding treatment are weakly dependent on the potentials applied on the specimens.
Formation of the soft magnetic nanostructure in amorphous Fe_1_4Ni_4_0Zr_7B_1_2 alloy due to heat treatment is studied by the Moessbauer, differential scanning calorimetry, and X-raydiffraction techniques. Annealing at temperatures 520-580 "oC leads to the formation of extremely soft nanocrystalline alloy as revealed by the rf-Moessbauer measurements. The superparamagnetic behaviour was observed for the alloy annealed at 620-640 "oC. At higher annealing temperatures good soft magnetic properties deteriorate. (author)
A mixture of powders of silica and aluminum nitride is subjected to high-energy ball milling for different milling times. This material is subsequently compacted by uniaxial pressing and sintered at 1450 deg. C. The resulting pellets are crushed and analysed by X-raydiffraction. For short milling times, the amount of phase transformation is minimal and the resulting material mostly consists of cristobalite and aluminum nitride. For long milling times, nanocrystalline #beta#-SiAl_2O_2N_2 is mainly produced.
(Pb_1_-_x La_x) (Zr_0_._6_5 Ti_0_._3_5) ceramics, with x = 0.09 (PLZT 9/65/35) were prepared using lead monoxide (Pb O) with different amount of litharge (tetragonal) and massicot (orthorhombic) phases. Results, based on x-raydiffraction patterns, remanent polarization and dielectric measurements, show that the Pb O polymorphic phase does not change the final structure of the PLZT but causes changes on the remanent polarization and dielectric permittivity temperature dependence. (author). 11 refs, 2 figs, 2 tabs.
The crystal structure and optical reflectivity of AlP has been studied in a diamond anvil cell using energy dispersive x-raydiffraction to 43 GPa and micro-optical reflectance spectroscopy to 36 GPa. AlP undergoes a first order phase transformation from zincblende to a NiAs structure which exhibits metallic reflectivity in the near-infrared. The decrease in volume on transformation is 17%[plus minus]1%. The transformation is reversible but has large hysteresis. The equilibrium transformation pressure is 9.5[plus minus]5 GPa.
AlN nanocrystalline layers and superstructures are used in the modern optoelectronic technology as reflecting mirrors in semiconductor layers. In the present work the properties of AlN films prepared by sputtering methods from an AlN target in reactive Ar + N plasma were investigated. The characterization was performed with HRTEM, SEM, glancing angle XRD and RBS methods. The present measurements confirmed the polycrystalline structure of AlN layers and enabled the evaluation of their grain size. The roughness and thickness of the layers were additionally determined by ellipsometric and profilometric measurements. (author)
Crystal structure of monoclinic telluric acid ammonium phosphate (TAAP) has been studied by an X-raydiffraction method in the paraelectric phase at 333 K and in the ferroelectric phase at room temperature. It is confirmed that the space group in the paraelectric phase is P2/n. Comparison of the results between the two temperatures suggests that the plane which is made by the PO{sub 4} tetrahedron linked by hydrogen bonds has an important role for the ferroelectric phase transition. This plane is almost parallel to the direction of spontaneous polarization.
This was a project to investigate the crystal chemistry of OH and H{sub 2}O substitution in silicate minerals by use of X-ray and neutron diffraction methods combined with IR spectroscopy and to interpret and generalize the results using an electrostatic model for these mineral structures. Using these data together with published H position data electrostatic parameters for H sites were calculated from a simple electrostatic model. The data were then used to refine the model for incorporation of H into the wadsleyite structure. This has led to recent work on the synthesis and characterization of hydrous wadsleyites.
The study is concerned with the combined effect of high pressure and shear strain on the properties of the A-15 intermetallics Nb3Sn and Nb3Al0.75Ge0.25. The properties discussed are the superconducting transition temperature, the width and intensity of the X-raydiffraction lines, and the width and shape of the Mossbauer absorption lines. It is shown that the combined effect of high pressure and shear strain leads to an intense generation of defects in polycrystalline specimens; the size of the ordered regions does not exceed 300 A even under the least severe conditions. 5 references.
The crystal and molecular structures of the anti-acquired immunodeficiency syndrome agent 3'-azido-3'-deoxythymidine (AZT) have been determined by x-raydiffraction. There are two crystallographically independent AZT molecules in the crystal asymmetric unit; they have similar conformation and differ primarily in the glycosyl torsion angle. Comparisons with a hydrated thymidylate structure indicate that the azido group does not significantly affect the gross conformational preference of the molecule. The comparisons also suggest possible functional roles for the azido group in enzyme binding.
Most of the investigations have a theoretical sustenance based on molecular simulation. The area of application of molecular simulation is very wide, in the Materials Technology Department assigned to the Applied Sciences Management have been treated problems about metallic nano structures, glasses, interfaces, and molecules, to sustain and to explain some of the experimental results. Energy calculations are carried out to determine minimum energy structures, for later on to carry out calculations of some of their properties; as well as the images simulation of Electron microscopy and X-raydiffraction. (Author)
In this paper we describe a Ni-Sn intermetallic material obtained via template electroplating synthesis. The structure and the morphology of this material are investigated by Xraydiffraction (XRD) and Scanning Electron Microscopy (SEM) analyses. We demonstrate that Ni-Sn behaves as a sub-micrometric electrode showing a favourable response when cycled in a lithium cell. The results here reported suggest that the template electroplating is a promising synthetic approach that can lead to an optimized structure and morphology of the Ni-Sn electrode, such as to confer it a role of a high capacity anode in advanced lithium ion batteries.
We report the synthesis of four diorganotin(IV) compounds of Schiff base pyruvic acid hydrazone derivatives formulated as [R2SnLY]2, where L1 is 2-SC4H3CON2C(CH3)CO2 with Y = CH3CH2CH2CH2OH, R = n-Bu (1); L2 is C6H5CON2C(CH3)CO2 with Y = CH3CH2OH, R = p-F-Bz (2); L3 is 2-HOC6H4CON2C(CH3)CO2 with YH2O, R = p-CN-Bz (3); and L4 is 4-NO2-C6H4CON2C(CH3)CO2 with YCH3CH2OH, R = Bz (4). The structures of all compounds have been established by a combination of single-crystal X-raydiffractionanalysis, 1H and 119Sn NMR spectroscopy, IR spectroscopy, and elemental analysis. Studies reveal that four ligands present the same coordination mode with tin center, which all present tridentate ONO donor Schiff bases and coordinate to the tin center in an enolic form. In compounds 1-4, each tin atom is seven...
A family of mixed LiCo{sub y}Ni{sub (1-y)}VO{sub 4} (y=0.2, 0.5 and 0.8) compounds of potential use as high voltage cathode materials in lithium batteries, has been synthesized and characterized. The X-raydiffractionanalysis showed that these compounds adopt an inverse spinel structure where in average 85% of the Ni{sup 2+} and Co{sup 2+} ions occupy octahedral sites and the other 15% occupy tetrahedral sites with the V{sup 5+} ions, although this occupation share is somewhat influenced by the preparation temperature. The annealing temperature plays also a key role in determining the particle size, as demonstrated by scanning electron microscope analysis. Cycling voltammetry tests showed that the lithium insertion-deinsertion process in the LiCo{sub y}Ni{sub (1-y)}VO{sub 4} electrode materials occurs reversibly around 4.3-4.4 V vs. Li, as also confirmed by cycling tests. The cycling capacity is ...
In this work, ZnO thin films have been grown on glass substrates by using a solution of propanol (C{sub 3}H{sub 8}O), water (H{sub 2}O) and zinc acetate (Z{sub n}(CH{sub 3}CO{sub 2}){sub 2}) in acidified medium (pH 5). The obtained films were n doped with ytterbium (Yb) at the rates of 100, 200 and 300 ppm. The structural features of the doped films were investigated using XRD, atomic force microscopy and scanning electronic microscopy techniques. XRD analysis shows a strong (0 0 2) X-raydiffraction line for increasing Yb-doping amounts. This c-axis preferential orientation of ZnO crystallites is naturally required to use this oxide as transparent conductor in optoelectronic applications. Atomic force microscopy (AFM) analysis shows an enhancement in the surface roughness of the doped ZnO:Yb thin films. Optical measurements were performed in 300-1800 nm domain via transmittance T(lambda) and ...
In this work, ZnO thin films have been grown on glass substrates by using a solution of propanol (C3H8O), water (H2O) and zinc acetate (Zn(CH3CO2)2) in acidified medium (pH 5). The obtained films were n doped with ytterbium (Yb) at the rates of 100, 200 and 300 ppm. The structural features of the doped films were investigated using XRD, atomic force microscopy and scanning electronic microscopy techniques. XRD analysis shows a strong (0 0 2) X-raydiffraction line for increasing Yb-doping amounts. This c-axis preferential orientation of ZnO crystallites is naturally required to use this oxide as transparent conductor in optoelectronic applications. Atomic force microscopy (AFM) analysis shows an enhancement in the surface roughness of the doped ZnO:Yb thin films. Optical measurements were performed in 300-1800 nm domain via transmittance T(?) and reflectance R(?) spectra. Conjoint optical and thermal ...
The nano-structured Fe(III)-doped TiO{sub 2} photocatalysts with anatase phase have been developed for the oxidation of non-biodegradable different organic dyes like methyl orange (MO), rhodamine B (RB), thymol blue (TB) and bromocresol green (BG) using UV-Hg-lamp. The different compositions of Fe{sub x}Ti{sub 1-x}O{sub 2} (x = 0.005, 0.01, 0.05, and 0.1) nanocatalysts synthesized by chemical method (CM), have been characterized by X-raydiffraction (XRD), UV-vis diffuse reflectance spectra, specific surface area (BET), transmission electronic microscopy (TEM) analysis, XPS, ESR and zeta potential. From XRD analysis, the results indicate that all the compositions of Fe(III) doped in TiO{sub 2} catalysts gives only anatase phase not rutile phase. For complete degradation of all the solutions of the dyes (MO, RB, TB, and BG), the composition with x = 0.005 is more photoactive compared all other ...
A geological study was conducted to better understand the nature of cleat development and degree of mineralization in coal seams of the Scollard and Coalspur Formations in western Alberta. The results can be applied to equivalent formations. The source and reservoir rocks of a coalbed methane (CBM) system were described. Coal seams are basically fractured reservoirs with 7 types of cleats. The field work involved cleat minerals sampling and determining cleat attributes such as type, strike and spacing from open-cut mines and outcrops. The laboratory work involved X-Raydiffraction, scanning electron microscopy, energy dispersive microscopy, stable isotope analysis, and fluid inclusions analysis. The study showed that coal seams of the Scollard and Coalspur Formations are widespread and cleated to various degrees. The face and butt cleats strike northeast-southwest and northwest southeast respectively ...
Red mud is a solid waste produced in the process of alumina extraction from bauxite. In this paper, recovery iron from Bayer red mud was studied with direct reduction roasting process followed by magnetic separation, and then building materials were prepared from alumosilicate residues. After analysis of chemical composition and crystalline phase, the effects of different parameters on recovery efficiency of iron were carried out. The optimum reaction parameters were proposed as the following: ratio of carbon powder: red mud at 18:100, ratio of additives: red mud at 6:100, roasting at 1300 deg. C for 110 min. With these optimum parameters, total content of iron in concentrated materials was 88.77%, metallization ratio of 97.69% and recovery ratio of 81.40%. Then brick specimens were prepared with alumosilicate residues and hydrated lime. Mean compressive strength of specimens was 24.10 MPa. It was indicated that main mineral phase transformed from nepheline ...
The use of the ratio of the characteristic intensity to the continuum background intensity (P/B ratio) of the X-ray spectrum for a quantitative ion microprobe (IMP) or PIXE (particle induced X-ray emission) analysis of thin biological specimens was proposed previously. The IMP analysis of thick biological specimens is also of considerable practical use. In this paper, the possibility of using the P/B ratio to quantify minor elements in thick biological specimens is investigated. The epoxy resin based standards with gradual concentrations of KCNS up to 0.6 mol/kg and NBS bovine liver were analyzed by a 27 MeV {alpha} particle microprobe. The measured peak to background ratios (between 4.4 to 5.7 keV) agreed well with the theoretical calculations. The calculations showed that the concentration dependence of the P/B ratios was determined mainly by the absorption of X-rays in specimens. ...
This volume of the monograph covers the following topics: activation analysis, non-activation interaction analysis (elastic scattering of charged particles, absorption and backscattering of beta radiation and photons, radionuclide X-ray fluorescence analysis, thermalization, scattering and absorption of neutrons, use of ionization caused by nuclear radiation, use of ionization by alpha or beta radiation for the measurement of pressure, density and flow rate of gases), and automation in radioanalytical chemistry. (P.A.).
Methods of sample treatment in XRF analysis of hair are studied in view of the effect on analytical results. A new method is proposed based on the incomplete ashing of hair followed by pellet preparation. Its suitability is estimated on the XRF analysis of real hair samples collected from 4 healthy adults. (author) 12 refs.; 4 figs.; 1 tab.
Full text of publication follows: Large-scale problems such as nuclear waste disposal are increasingly recognized to be interconnected to small scale-mechanisms. Thus, synchrotron-based high-resolution analytical X-ray probes become important tools for exploring the micro-scale chemical reactivity of heterogeneous barrier materials used in nuclear waste repositories. In this study the layout of the micro-XAS beamline at the Swiss Light Source (SLS) will be presented. The beamline is optimized towards micro beam experiments ({approx}1 x 1 {mu}m{sup 2}) in the hard-X-ray regime (4 - {approx}22 keV) and allows to combine micro X-ray fluorescence (micro-XRF), micro X-ray absorption spectroscopy (micro- XAS), and micro X-raydiffraction (micro-XRD) investigations with radioactive samples. Furthermore, the potential of micro-XRF/XAS/XRD for acquiring spatially ...
Radionuclide X-ray fluorescence analysis for nondestructive determination of Fe, Zn, Pb, and Br in air samples collected on nitrocellulose membrane filter Synpor 4 is described. A /sup 238/Pu source for the excitation and a semiconductor Si/Li detector for the detection of characteristic and L-fluorescent radiation of the above elements were used. A correction method based upon the measurements of simple or multiple Compton scattering for compensation of varying mass per unit area values in sample deposits was theoretically proposed and experimentally tested. The results obtained both with and without the correction were compared and good agreement with those given by atomic absorption spectrometry was observed.
The purpose of the present study is to develop a new method for chemical state analysis by means of EPMA(Electron probe microanalyser). The measured X-ray intensity of Si-K{beta} characteristic X-ray spectra were read-out by a 16 bit microcomputer with a RS-232C interface. And using the curve fitting method the quantitative analysis of chemical compositions in a ternary compound that constituted of the same element has been established. The present method was applied to analyse of the friction and wear properties of Si-base ceramics sliding materials. It was found that the wear debris contains both the compositions of the sliding materials and SiO{sub 2}, and the SiO{sub 2} contents in wear debris was changed with relative humidity. The results clearly showed that the proposed method is very useful for determing the compositions in the ternary compound. (author).
The purpose of the present study is to develop a new method for chemical state analysis by means of EPMA(Electron probe microanalyser). The measured X-ray intensity of Si-K#beta# characteristic X-ray spectra were read-out by a 16 bit microcomputer with a RS-232C interface. And using the curve fitting method the quantitative analysis of chemical compositions in a ternary compound that constituted of the same element has been established. The present method was applied to analyse of the friction and wear properties of Si-base ceramics sliding materials. It was found that the wear debris contains both the compositions of the sliding materials and SiO_2, and the SiO_2 contents in wear debris was changed with relative humidity. The results clearly showed that the proposed method is very useful for determing the compositions in the ternary compound. (author).
We present a fully automated method for three-dimensional (3D) elemental analysis demonstrated using a ceramic sample of chemistry (Ca)MgTiO_x. The specimen is serially sectioned by a focused ion beam (FIB) microscope, and energy-dispersive X-ray spectrometry (EDXS) is used for elemental analysis of each cross-section created. A 3D elemental model is reconstructed from the stack of two-dimensional (2D) data. This work concentrates on issues arising from process automation, the large sample volume of approximately 17x17x10 #mu#m"3, and the insulating nature of the specimen. A new routine for post-acquisition data correction of different drift effects is demonstrated. Furthermore, it is shown that EDXS data may be erroneous for specimens containing voids, and that back-scattered electron images have to be used to correct for these errors.
Alloy 800 and Alloy 600 are well known for their resistance to corrosion in an aqueous medium at high pressure and temperature, for which they have been widely used for more than 3 decades in different structural components of water refrigerated nuclear reactors, especially as material for the steam generator tubes (SG) in these nuclear plants. The SG tubes in the Atucha I and Embalse Nuclear Plants are made with Alloy 800. The speed of corrosion of these materials in a reactor's refrigerant medium, while very small is perfectly measurable and can be described by parabolic or logarithmic type kinetics. In other words this speed is high in the first states of growth during the formation of a protective oxide film but then drops to almost stationary values. One characteristic of these films is the formation of a double layer (or duplex): i) an internal adhering layer, of approximately constant thickness, formed by small microcrystals (#<=#0.05 mm), ii) a less adhering external one, ...
X-raydiffraction enhanced imaging (DEI) is applied to inspect internal structures of weakly absorbing low-Z sample. How to extract phase information from raw images measured in different positions of rocking curve is the key problem of DEI. In this paper, we present an effective extraction method called polynomial curve fitting method, in order to extract accurate information angular in a fast speed. It is com- pared with the existing methods such as multiple-images statistical method and Gaussian curve fitting method. The experiments results on a plastic cylinder and a black ant at the Beijing Synchrotron Radiation Facility prove that the polynomial curve fitting method can obtain most approximate refraction-angle values and its computation speed is 10 times faster than the Gaussian curve fitting method. (authors)
Heusler films with L2_1 and B2 structure are deposited simultaneously on amorphous carbon films, Si(100) surfaces, and in situ cleaved InAs(110) surfaces by coevaporation of Ni and the alloy MnIn. Morphology, structure, and stoichiometry are investigated with transmission-electron microscopy, electron diffraction, and X-ray spectroscopy. The almost perfect lattice match supports highly oriented growth of Ni_2MnIn on InAs, which is proven by electron diffraction under grazing incidence. The electrical resistivity of thin films on Si show metallic behavior. At temperatures of liquid helium point-contact Andreev reflection spectroscopy is performed on films grown on Si(100) and in situ cleaved InAs(110) surfaces yielding spin polarizations comparable to the ones of Fe, Ni, Co, and permalloy (Ni_8_0Fe_2_0).
The structure of nano-porous carbon, obtained by means of chlorination of carbide compounds with various crystal structure (SiC, TiC, Mo_2C) is studied through the method of small-angle diffraction. The angular dependences of the scattering intensity obtained are interpreted as the result of scattering from the nanoparticles of different size. The functions of the scattering particles distribution by the m(R_g) inertia radii are determined. It is shown that in spite of the source carbide, the highest fraction of the volume in the porous carbon constitute the particles with R_g #approx# 5 A. The nanoparticles in the samples obtained from SiC, wherein the average value of the R_g"a"v < 6 A, are most uniform by size. The nanoparticles in the porous carbon, obtained from Mo_2C, are on the average by two times larger
The microstructure of commercial rolled magnesium alloy AZ31B (nominal composition Mg-3Al-0.9Zn-0.15Mn in wt.%) was investigated with the help of light microscopy, electron backscatter diffraction (EBSD) and X-raydiffraction technique after annealing in the temperature range from room temperature (RT) to 400 deg. C. Tensile tests at RT were performed to show the influence of the microstructure on mechanical properties. Static recrystallization (SRX) was observed during annealing of as-received alloy at and above 150 deg. C. Twins play an important role during SRX and serve as nucleation sites and preferred paths for growth of grains. The strong basal texture caused by rolling was weakened by SRX. Significant differences in the stress strain curves were observed for as-received and annealed specimens.
With the deposition of PVD hard coatings on the tools applied in machining operations it is possible to achieve significant improvements in the performance and quality of the machining processes. Depending on the machined material and the operating principle, e.g. turning, milling or drilling, not only different machining parameters but also different coating materials are necessary. In interrupted cut machining of tempered steel, for example, the life time of Ti-C-N coated inserts is several times greater than the Ti-C-N coated ones. This is a result of the favourable thermophysical and tribological properties of Ti-N-C. The potential for tool protection by CrN coatings is a result of the high ductility and low internal stress of this coating materials. CrN films can be deposited with greater film thickness, still maintaining very good adhesion. This paper presents the development of new arc PVD coatings in the system Cr-C-N. Owing to the carbon content in the coating an increased ...
On the basis of accurate crystal structure determination, the mineral phosphuranylite corresponds to the chemical formula KCa(H_3O)_3(UO_2)_7(PO_4)_4O_4.8H_2O. Cmcm, a=15.778 (3)-15.899(2), b=13.702(2)-13.790(5), c=17.253(3)-17.330(3)A, Z=4, D_x=4.575-4.631g cm"-"3, #mu#=287.6-291.1cm"-"1. The presence of potassium (about 1.80wt%K_2O), overlooked until now, has been confirmed by microprobe analysis on samples from four different localities. The best data for structure determination have been obtained by single-crystal X-raydiffraction on specimens from Capoterra, Sardinia, and Bois Noirs, France; here 1453 and 1254 independent reflections, respectively, were used in the refinement, and the corresponding final R index is 0.036 and 0.048. The structure consists of layers of phosphate groups connected with hexagonal, pentagonal and tetragonal dipyramids centered on the U atoms. The Ca and K atoms are located within channels ...
A WO(3)/TiO(2) composite, hollow-sphere photocatalyst with average diameter of 320 nm and shell thickness of 50 nm was successfully prepared using a template method. UV-vis diffuse reflectance spectra illustrated that the main absorption edges of the WO(3)/TiO(2) hollow spheres were red-shifted compared to the TiO(2) hollow spheres, indicating an extension of light absorption into the visible region of the composite photocatalyst. The WO(3) and TiO(2) phases were confirmed by X-raydiffractionanalysis. BET isotherms revealed that the specific surface area and average pore diameter of the hollow spheres were 40.95 m(2)/g and 19 nm, respectively. Photocatalytic experiments indicate that 78% MB was degraded by WO(3)/TiO(2) hollow spheres under visible light within 80 min. Under the same conditions, only 24% MB can be photodegraded by TiO(2). The photocatalytic mineralization of MB, catalyzed by TiO(2) and WO(3)/TiO(2), ...
A new iron phosphate (NH4)4Fe3(OH)2F2[H3(PO4)4] has been synthesized hydrothermally at HF concentrations from 0.5 to 1.2 mL. Single-crystal X-raydiffractionanalysis reveals its three-dimensional open-framework structure (monoclinic, space group P21/n (No. 14), a=6.2614(13) A, b=9.844(2) A, c=14.271(3) A, ?=92.11(1)o, V=879.0(3) A3). This structure is built from isolated linear trimers of corner-sharing Fe(III) octahedra, which are linked by (PO4) groups to form ten-membered-ring channels along [1 0 0]. This isolated, linear trimer of corner-sharing Fe(III) octahedra, [(FeO4)3(OH)2F2], is new and adds to the diverse linkages of Fe polyhedra as secondary building units in iron phosphates. The trivalent iron at octahedral sites for the title compound has been confirmed by synchrotron Fe K-edge XANES spectra and magnetic measurements. Magnetic measurements also show that this compound exhibit a strong antiferromagnetic ...
Abstract A series of small phosphazene ligands with pendant 6-phenyl-2,2--bipyridyl moieties, namely L1 [N3P3(OPh)5(OPhbpyPh)], L2 [N3P3(biph)2(OPhbpyPh)2], L3 [N3P3(tBubiph)2(OPhbpyPh)2], L4 [N3P3(biph)2(OPhbpyPh)Cl] and L5 [N3P3(biph)2(OPhbpyPh)(OPh)] [OPhbpyPh = 4-(4-phenoxy)-6-phenyl-2,2--bipyridine, OPh = phenoxy, biph = 2,2--oxybiphenyl and tBubiph = 4,4--di-tert-butyl-2,2--oxybiphenyl], have been used to synthesise the new cyclometallated palladium(II) and platinum(II) complexes [(L1-H)PdCl], [(L1-H)PtCl], [(L1-H)(PdCl)2], [(L3-H)(PdCl)2], [(L4-H)PtCl], [(L5-H)PtCl] and the rhenium(I) complex [L5Re(CO)3Cl]. Single-crystal X-raydiffractionanalysis was performed on the free ligand L2 and the palladium complexes [(L1-H)PdCl] and [(L3-H)(PdCl)2]. In both PdII complexes, the metal cent...
In this paper, we present the photoluminescence properties of Pr3+-, Sm3+- and Dy3+-doped germanate glasses and glass ceramics. From the X-raydiffraction measurement, the host glass structure was determined. These glasses have shown strong absorption bands in the near-infrared (NIR) region. Compared to Pr3+-, Sm3+- and Dy3+-doped glasses, their respective glass ceramics have shown stronger emissions due to the Ba2TiGe2O8 crystalline phase. For Pr3+-doped glass and glass ceramic, emission bands centered at 530nm (3P03H5), 614nm (3P03H6), 647nm (3P03F2) and 686nm (3P03F3) have been observed with 485nm (3H43P0) excitation wavelength. Of them, 647nm (3P03F2) has shown bright red emission. Emission bands of 4G5/26H5/2 (565nm), 4G5/26H7/2 (602nm) and 4G5/26H9/2 (648nm) for the Sm3+:glass and gl...
Single phase amorphous Al_xHf_1_0_0_-_x alloys with a wide amorphization range (33#<=#x#<=#75) were synthesized by the solid-state interdiffusion of pure polycrystalline Al and Hf powders at room temperature using a rod-milling technique. The mechanisms of metallic glass formation and competing crystallization processes in the mechanically deformed composite powders were investigated by means of X-raydiffraction, differential thermal analysis, scanning electron microscopy and transmission electron microscopy. The numerous intimate layered composite particles of the diffusion couples that formed during the first and intermediate stages of milling (0-173 ks) are intermixed to form amorphous phase(s) upon heating to about 980 K by so-called thermally assisted solid-state amorphization (TASSA). The amorphization heat formation for the binary Al_xHf_1_0_0_-_x system via TASSA, #DELTA#H"T"A"S"S"A_a, was measured directly ...
Ti and its alloys (Ti-6Al-4V) have been used in different engineering applications due to their several outstanding properties. Nevertheless, their use in practical applications is limited in many cases due to their poor tribological property. Researches are ongoing on surface modification of Ti based materials by different plasma and ion based techniques to overcome this problem. However, the conventional plasma nitriding techniques have several problems such as formation of an arc, increased possibility of surface contamination due to a comparatively higher operating pressure, production of a very thin nitrided layer after a long processing time, etc. In this present work, the possibility of a new low-pressure plasma nitriding process using a Plasma Enhanced Chemical Vapor Deposition (PECVD) based saddle field fast atom beam source on a Ti-6Al-4V alloy sample is investigated. Plasma nitriding was carried out at 900 deg. C and at a pressure 0.1 Pa for 8 h by using a beam current 0.5 ...
Ti and its alloys (Ti-6Al-4V) have been used in different engineering applications due to their several outstanding properties. Nevertheless, their use in practical applications is limited in many cases due to their poor tribological property. Researches are ongoing on surface modification of Ti based materials by different plasma and ion based techniques to overcome this problem. However, the conventional plasma nitriding techniques have several problems such as formation of an arc, increased possibility of surface contamination due to a comparatively higher operating pressure, production of a very thin nitrided layer after a long processing time, etc. In this present work, the possibility of a new low-pressure plasma nitriding process using a Plasma Enhanced Chemical Vapor Deposition (PECVD) based saddle field fast atom beam source on a Ti-6Al-4V alloy sample is investigated. Plasma nitriding was carried out at 900 deg. C and at a pressure 0.1 Pa for 8 h by using a beam current 0.5 ...
Investigations of alternative renewable energy resources continue, with many studies concentrating on hydrogen storage. However, there are a few problems such as storage, transportation, delivery to the user and usage safely, to be addressed to facilitate commercialization and wide usage of the hydrogen. The absorbed form within the metal hydrides seems to be the best solution of this problem. Since Li is the lightest metal, it has the advantage as the stored amount of hydrogen mass ratio. LiBH{sub 4} production process was investigated using elemental Li, B and H{sub 2}. Spex type ball milling with tungsten carbide, stainless steel and zirconia type vessels, was used to mix the different amount of Li and B under argon atmosphere. X-raydiffraction pattern demonstrated that the LiB was obtained. A system was designed to provide a hydrogen atmosphere of 60 bars to force hydrogen into the LiB structure. FTIR analysis strongly ...
The U.S. Geological Survey, in cooperation with the U.S. Department of Energy, is conducting a study to determine the natural geochemistry of the Snake River Plain aquifer system at the Idaho National Engineering Laboratory (INEL), Idaho. As part of this study, a group of geochemical reactions that partially control the natural chemistry of ground water at the INEL were identified. Mineralogy of the aquifer matrix was determined using X-raydiffraction and thin-section analysis and theoretical stabilities of the minerals were used to identify potential solid-phase reactants and products of the reactions. The reactants and products that have an important contribution to the natural geochemistry include labradorite, olivine, pyroxene, smectite, calcite, ferric oxyhydroxide, and several silica phases. To further identify the reactions, analyses of 22 representative water samples from sites tapping the Snake River Plain aquifer ...
Crystalline and non-crystalline iron oxide (#alpha#-Fe_2O_3) thin films were obtained by spray pyrolysis onto glass substrate at different temperatures. The results of X-raydiffraction showed that with increasing the deposition time, the film structure changed from non-crystalline to crystalline at the same substrate temperature. At different substrate temperatures and low deposition times (5 min), iron oxide appears almost in non-crystalline form. With rising the substrate temperature and deposition time, the crystallinity was improved. The effect of substrate temperature as well as deposition time on the optical features (absorption coefficient and bandgap) and optical constants of these films has been investigated. Optical constants of the films were determined from spectrophotometric measurement of reflectance and transmittance. Analysis of the results showed that, for non-crystalline iron oxide films of different ...
The ternary compound CuInS{sub 2} is attractive for solar cells due to its band gap of 1.54 eV which borders the optimum value necessary for conversion of a solar spectrum. Recently, works on thin film cells based on this material (ZnO/CuInS{sub 2}) has been reported to show efficiency as high as 11.4%. In this paper, the orientation and the morphology of CuInS{sub 2} sprayed films are determined by the means of X-raydiffraction and scanning electron microscopy. Sprayed CuInS{sub 2} films deposited onto a transparent Pyrex substrate with standard fabrication parameters show a chalcopyrite structure with a preferential orientation (1 1 2). A model based on the calculation of the relative dielectric function {epsilon} has been performed in order to obtain the profile of variation of this parameter and to understand the optical behavior of this material via its transmittance and reflectance in visible and near-infrared regions (0.35-2.5 {mu}m). ...
The ternary compound CuInS2 is attractive for solar cells due to its band gap of 1.54 eV which borders the optimum value necessary for conversion of a solar spectrum. Recently, works on thin film cells based on this material (ZnO/CuInS2) has been reported to show efficiency as high as 11.4%. In this paper, the orientation and the morphology of CuInS2 sprayed films are determined by the means of X-raydiffraction and scanning electron microscopy. Sprayed CuInS2 films deposited onto a transparent Pyrex substrate with standard fabrication parameters show a chalcopyrite structure with a preferential orientation (1 1 2). A model based on the calculation of the relative dielectric function ? has been performed in order to obtain the profile of variation of this parameter and to understand the optical behavior of this material via its transmittance and reflectance in visible and near-infrared regions (0.35-2.5 ?m). In the same way, considering the ...
A mesoscopically ordered lamellar gel phase of a polymer-grafted, lipid-based complex fluid is used as a scaffolding to spatially organize inorganic nanoparticles. The complex fluid provides both a highly anisotropic environment and a segregated aqueous and organic domains in which inorganic nanoparticles can be selectively placed by tailoring their size and surface characteristics. Three types of silver nanoparticles -- underivatized, surfactant-stabilized, and dodecanthiol-derivatized -- were evaluated. Comparison of the surface plasmon resonance of the various silver particles dispersed in conventional solvents to those contained within the complex fluid was used to determine the region of spatial localization in the lamellar gel phase. Silver particles rendered hydrophobic by capping with an alkane thiol insert into the hydrocarbon bilayer region. Surfactant-stabilized and underivatized silver nanoparticles reside in the aqueous channels, with the latter particles preferentially ...
The valence and spin-state distributions of Co ions and the complex structure of antiferromagnetic Ba_2Co_9O_1_4 have led to the suggestion that doped Ba_2Co_9O_1_4 compounds may be good thermoelectric materials. We have checked this suggestion by measuring the magnetic properties as well as the transport properties of nominal Ba_1_._9A_0_._1Co_9O_1_4 (A=La or Na). We show that although all compounds are indicated to be single phase by powder X-raydiffractionanalysis, they are all p-type polaronic conductors with low mobile-hole concentrations. Magnetic-susceptibility data of the parent and La-doped compounds give evidence of a second magnetic phase with ferromagnetic order setting in below 215 K; but this second phase is not seen in the Na-doped sample. We conclude that the structure is stabilized by oxidation and that cation exolution from the Ba_2Co_9O_1_4 structure creates cation vacancies that oxidize the high-spin ...
The effect of thermal pretreatment in N[sub 2] up to 723 K and the activation treatments in H[sub 2] and an inert atmosphere on the properties of Ni and Co activated-charcoal-supported catalysts were studied. Catalysts were characterized by means of N[sub 2] adsorption at 77 K, H[sub 2] chemisorption at room temperature, thermogravimetric analysis (TGA), X-raydiffraction (XRD), and transmission electron microscopy (TEM). The catalysts' activity and selectivity for acetone hydrogenation to 2-propanol under unusual and severe conditions (473 K and high overall acetone conversion) were also measured. TGA and XRD evidence was found for the charcoal-support-promoted NiO and CoO reduction to the metallic states when the catalysts were subjected to an inert atmosphere above 723 K caused a loss of acetone hydrogenation activity (calculated on a metal load basis) for both the Ni and Co activated-charcoal-supported ...
Chemical looping combustion (CLC) of simulated coal-derived synthesis gas was conducted with NiO oxygen carriers supported on SiO2, ZrO2, TiO2, and sepiolite. The effect of H2S on the performance of these samples for the CLC process was also evaluated. Five-cycle thermogravimetric analysis (TGA) tests at 800 C indicated that all oxygen carriers had a stable performance at 800 C, except NiO/SiO2. Full reduction/oxidation reactions of the oxygen carrier were obtained during the five-cycle test. It was found that support had a significant effect on reaction performance of NiO both in reduction and oxidation rates. The reduction reaction was significantly faster than the oxidation reaction for all oxygen carriers, while the oxidation reaction is fairly slow due to oxygen diffusion on NiO layers. The reaction profile was greatly affected by the presence of H2S, but there was no effect on the capacity due to the presence of H2S in synthesis gas. The presence of H2S ...
CuO/bentonite and CuO-BHA nanocomposites were studied as oxygen carriers in chemical-looping combustion (CLC) of simulated synthesis gas. Global reaction rates of reduction and oxidation, as the function of reaction conversion, were calculated from 10-cycle oxidation/reduction tests utilizing thermogravimetric analysis at atmospheric pressure between 700 and 900{degree}C. It was found that the reduction reactions are always faster than oxidation reactions; reaction temperature and particle size do not significantly affect the reaction performance of CuO/bentonite. Multicycle CLC tests conducted in a high-pressure flow reactor showed stable reactivity for production of CO{sub 2} from fuel gas at 800 and 900{degree}C and full consumption of hydrogen during the reaction. Results of the tapered element oscillating microbalance showed a negative effect of pressure on the global rates of reduction-oxidation reactions at higher fractional conversions. ...
Immobilization of a model liquid organic pollutant, i.e. the 2-chloroaniline (2-CA), into a cement matrix using organoclays as pre-sorbent agents was investigated. Five cement-clay pastes were prepared with different nominal water-to-cement ratios (w/c=0.40, 0.25 and 0.15 wt/wt) and various amounts of waste (waste-to-cement o/c=0.20, 0.60 and 1.00 wt/wt); for comparison, a neat cement paste was also prepared. Dynamic leach tests were performed on solidified monoliths in order to assess the successful immobilization of the 2-CA. In monoliths at constant w/c ratio (0.40) the total amount of pollutant released increases with its initial content, and ranges from 15 to 35% with respect to it. By lowering w/c from 0.40 to 0.15 at constant o/c, the performances improved (<25% released). The microstructure of the hardened cement-clay pastes was characterized by quantitative X-raydiffraction (QXRD) and electronic microscopy (SEM-EDS) techniques; ...
A way to synthesize the transient zwitterionic silylene L'Si: 8 {L'=CH[(C=CH(2))CMe(N(tBu))(2)]} and achieve its facile dimerization to the remarkable N-heterobicyclic disilane 8(2) is described. At first, employing the beta-diketiminate ligand L [L=CH(CMeN(tBu))(2)], both starting materials LH (2) and its N-lithium salt LLi (3) can react with SiBr(4) to yield the silylene precursor L'SiBr(2) (4) by silicon-induced C-H activation at an exocyclic methyl group on the backbone of the ligand. Compound 4 reacts with SiBr(4) above room temperature to afford the unexpected terminal CH(SiBr(3))-substituted dibromosilane 6 along with the unique tricyclic trisilane 7. Reduction of 4 with KC(8) at 0 degrees C furnishes the novel N-heterobicyclic disilane 8(2), which is a formal dimer of the desired zwitterionic silylene L'Si: (8). It has been reasoned that compound 8(2) may results from [4+1] cycloaddition of two molecules of 8 to give the transient dimer 8(2)', which subsequently undergoes ...
We have performed extended X-ray absorption fine structure (EXAFS) analysis for artificial Cr-goethite to elucidate the local structure around Cr in Cr-goethite. The spectra were obtained using synchrotron radiation X-rays at the Photon Factory in Tsukuba. The first shell contributions were isolated by Fourier filtering EXAFS data, and the inverse Fourier transformed single-shell data were analyzed using a curve fitting method. The results show that Cr is coordinated with (7#+-#1)O"2"- ions. The protective characteristics of the Cr-goethite protective rust layer on weathering steel can be interpreted in terms of the O"2"- coordination around Cr"3"+ resulting in the creation of negative fixed charge in the Cr-goethite particles. (author)
Double-crystal high-resolution X-ray fluorescence spectrometry was applied to the state analysis of sulfur in coal and related fly ash. For total sulfur, a proportional relationship exists between fluorescence intensities and the analytical values obtained by the oxygen-combustion method. Two oxidation states of sulfur were identified by a least square curve fitting method, by assuming that the spectrum profile is identical for each sulfur state but the intensity and the position are different. Sulfur in coal mainly consists of S/sup 2 -/, whereas that in coal fly ash mainly consists of S/sup 6 +/. As much as 0.04-0.08% of S/sup 2 -/ remains in fly ash.
In situ X-Ray microtomography offers new opportunities for analysing sintering mechanisms since it allows 3D observation of the microstructural evolution of the powder all along a sintering cycle. With synchrotron radiation at ESRF, a 3D image with a resolution of 2 {mu}m can be obtained in about one minute. In addition to the visual examination of the images, relevant microstructural parameters can be measured through quantitative image analysis using recently developed tools. In this paper the results obtained with two materials, loose copper powder and compacted steel powder, are resumed. For copper powder, the dispersion of local parameters such as particle co-ordination number and porosity is investigated. Concerning steel compacts, data about pore morphology evolution and on local strains provides clues for understanding the anisotropic shrinkage of such compacts. (authors)
This paper aimed to the evaluation of different kinds of sorbent material preparation and to the evaluation of their characteristics at different pH conditions by X-ray fluorescence analysis. This method is suitable for identification and determination of elements in samples of different character, state and origin because it is a polycomponent, non-destructive, fast and simple analytical method. Moreover, it allows timeadvantageous and reliable measurements. This paper studies problems concerning the determination of some selected elements (Mn, Fe, Ni, Cu, Zn, Pb) in pharmaceutical samples of sodium chloride in the solid state as well as in its solution by sorption on chelating extraction membrane 3M Empore"T"M and on the strongly acidic ion-exchanger Dowex 50Wx8. Conditions for the most effective sorption of determined elements are also interpreted. (author)
This paper aimed to the evaluation of different kinds of sorbent material preparation and to the evaluation of their characteristics at different pH conditions by X-ray fluorescence analysis. This method is suitable for identification and determination of elements in samples of different character, state and origin because it is a polycomponent, non-destructive, fast and simple analytical method. Moreover, it allows time-advantageous and reliable measurements. This paper studies problems concerning the determination of some selected elements (Mn, Fe, Ni, Cu, Zn, Pb) in pharmaceutical samples of sodium chloride in the solid state as well as in its solution by sorption on chelating extraction membrane 3M Empore? and on the strongly acidic ion-exchanger Dowex 50Wx8. Conditions for the most ef...
By dissolution of iron (2) carbonate in rhenium acid iron (2) perrhenate of the Fe(ReO/sub 4/)/sub 2/x4H/sub 2/O composition is obtained. By the method of thermal analysis the limits of tetra-, dihydrate and anhydrous iron (2) perrhenate stability are revealed. By means of Xray phase and IR spectroscopic analysis methods modification of structure in the process of synthesized salt dehydration is shown.
Technological processes of welding are significant sources of pollution in the working area. Evaluation of chemical quality of working area was made by means of radionuclide x-ray fluorescence analysis and activation analysis with fast neutrons. Welding aerosols were sampled by filtration method on Synpor 4 membrane ultra-filters. For selected types of welding filter metals, determination of heavy metals in aerosols was performed. (author).
Technological processes of welding are significant sources of pollution in the working area. Evaluation of chemical quality of working area was made by means of radionuclide x-ray fluorescence analysis and activation analysis with fast neutrons. Welding aerosols were sampled by filtration method on Synpor 4 membrane ultra-filters. For selected types of welding filter metals, determination of heavy metals in aerosols was performed.
An energy sensitive Si(Li) detector XRF analyzer built by ATOMKI, Hungary, has been applied for various analytical purposes in alumina production at the Almasfuezitoe Alumina Company, Hungary. Specifically, the CaO content in red mud was determined by the new XRF technique using isotope excitation sources. The analysis of other components is under way. (R.P.).
Proceeding from commercially available instruments, a simple measuring system has been established, which renders possible fast and simple discontinuous analysis of individual elements. This measuring system is described, giving some examples of utilization in nonferrous metallurgy (mining, ore dressing, metallurgical treatment), and specific details, such as error of measurement, ranges of measurement and limits of utilization. (author).
This article provides a survey of neutron scattering experiments in condensed matter research, which are of interest to chemistry. The theoretical background has been treated in a previous issue. The present article consists of two parts. The first part exhibits the range of experimental possibilities by means of a few selected examples. The starting point is classical neutron diffraction by which the position of atomic nuclei may be determined. Additional information on the spatial distribution in the outer electron shells may be obtained via combined X-ray/neutron-diffraction experiments or via the diffraction of polarized neutrons. Progress in instrumentation, due to the development of more intense sources, has influenced especially the fields of small angle scattering and spectroscopy. The second part features domains of research of current interest, where a combination of several neutron scattering techniques may prove ...
Radionuclide X-ray fluorescence analysis is a method, which has many advantages for analysing various historic artefacts, as it is relatively cheap, sensitive and non-destructive, and it allows measurements in-situ. However, this analysis has also certain limitations especially concerning sensitivity to chemical elements only, irrespective of the compounds or chemical forms in which these elements have been bonded. In addition, light elements emitting very soft X-rays cannot be measured, and in order to detect a wide range of elements, it is necessary to carry out repeated measurements with different radiation sources. Despite these limitations, valuable information can be obtained about the composition of historic materials and data about the origin and age of these artefacts can be derived. Analyses of wall paintings, ancient metal sculptures or other objects of art provide the basis for historic ...
Radionuclide X-ray fluorescence analysis is a method, which has many advantages for analysing various historic artefacts, as it is relatively cheap, sensitive and non-destructive, and it allows measurements in-situ. However, this analysis has also certain limitations especially concerning sensitivity to chemical elements only, irrespective of the compounds or chemical forms in which these elements have been bonded. In addition, light elements emitting very soft X-rays cannot be measured, and in order to detect a wide range of elements, it is necessary to carry out repeated measurements with different radiation sources. Despite these limitations, valuable information can be obtained about the composition of historic materials and data about the origin and age of these artefacts can be derived. Analyses of wall paintings, ancient metal sculptures or other objects of art provide the basis for historic ...
The Schiff base ligand, 4-isopropylbenzaldehyde[N-(3-oxo-3,4-dihydro-2-quinoxalinyl)hydrazone] (Ipbh), the 1:1 condensation product of 4-isopropylbenzaldehyde and 2-hydroxy-3-hydrazinoquinoxiline, has been synthesized and characterized by X-ray crystallography. A series of complexes of Ipbh with Nickel(II), viz., [Ni(Ipbh)2]Cl2 (1), [Ni(Ipbh)2]Br2 (2), [Ni(Ipbh)2]I2 (3), [Ni(Ipbh)2(CH3OH)2](NO3)2(CH3OH)2 (4) and [Ni(Ipbh)2ClO4]ClO4 (5) have been synthesized. All the complexes were characterized by elemental analysis, molar conductivity, CHN analysis, spectroscopic studies, magnetic susceptibility measurements and TG/DTA methods. The solid-state structure of the complex 4 was established by single crystal X-ray crystallography. In all the complexes, Ipbh acts as a bidentate NO chelating age...
We introduce a methodology for analysis of multiwavelength data from X-ray selected BL Lac (XBL) objects detected in the TeV regime. By assuming that the radio--through--X-ray flux from XBLs is nonthermal synchrotron radiation emitted by isotropically-distributed electrons in the randomly oriented magnetic field of a relativistic blazar jet, we obtain the electron spectrum. This spectrum is then used to deduce the synchrotron self-Compton (SSC) spectrum as a function of the Doppler factor, magnetic field, and variability timescale. The variability timescale is used to infer the comoving blob radius from light travel-time arguments, leaving only two parameters. With this approach, we accurately simulate the synchrotron and SSC spectrum of flaring XBLs in the Thomson through Klein-Nishina regimes. Photoabsorption by interactions with internal jet radiation and the intergalactic background light (IBL) is included. Doppler ...
An X-ray fluorometric train was set up for analyzing gravitational fallout, and tested on standard reference samples of fly ashes from conventional power plants. Analysis of thin layers proved inappropriate, and therefore pelletization of the samples, either alone or together with the X-ray MIX binder, was applied. Sample grinding in an agate mortar was found sufficient to suppress the particle size effect. The optimum pressure was 20 MPa. The optimum geometry was sought for "1"0"9Cd source, and limits of detection of 2.78-0.47 #mu#g were achieved for Cr-Zr elements. Tominaga's method was employed for matrix effect correction. Ti, Fe, Cu, Zn, As, Rb, Sr, Zr and Pb were determined in the SRM's; the relative errors ranged from units per cent (for Zn, Rb, Sr and Zr present in concentrations about 100 ppm and for Fe in concentrations of units per cent) up to 45% (for Ti present in a concentration of 0.67%). The method developed ...
The influence of a decarburisation process during austenitising of the through-hardenable rolling bearing steel 100Cr6 (SAE 52100) on the rim zone properties of the martensitic through-hardened material was investigated by means of material analysis and diffusion calculations. For this purpose, two specimens were prepared under defined heat treatment conditions, and the near-surface carbon distribution was determined micro-chemically by using secondary ion mass spectrometry (SIMS). In part 1 of the present work, these concentration profiles are compared with the depth variation of the micro-hardness and with the distance curves of the residual stresses and the line broadening ({l_brace}211{r_brace} {alpha}'-Fe diffraction line) both measured by X-raydiffraction (XRD). In addition, microstructure investigations were performed. In part 2, a refined kinetics model of a diffusion-controlled ...
An x-ray zone plate was fabricated using the novel approach of focused ion beam (FIB) milling. The FIB technique was developed in recent years, it has been successfully used for transmission electron microscopy (TEM) sample preparation, lithographic mask repair, and failure analysis of semiconductor devices. During FIB milling, material is removed by the physical sputtering action of ion bombardment. The sputter yield is high enough to remove a substantial amount of material, therefore FIB can perform a direct patterning with submicron accuracy. The authors succeeded in fabricating an x-ray phase zone plate using the Micrion 9500HT FIB station, which has a 50 kV Ga{sup +} column. Circular Fresnel zones were milled in a 1.0-{micro}m-thick TaSiN film deposited on a silicon wafer. The outermost zone width of the zone plate is 170 nm at a radius of 60 {micro}m. An achieved aspect ratio was 6:1.
A Real-Time Neutron Radiography (RTNR) system and a high speed X-ray Computed Tomography (X-CT) system are used to determine the flow regime, the instantaneous cross-sectional averaged void fraction, and the time averaged void fraction in a vertical annulus flow channel. A standard optical video system is also used to observe the flow regime. The annulus flow channel is operated as a bubble column and measurements are obtained for gas flow rates form 0.0 to 30.0 l/min. The flow regimes observed by all three measurement systems via image analysis shows that the results agree well with each other. Both the RTNR and the X-CT systems show that the time averaged and cross-sectional averaged void fraction increases with increasing superficial gas velocity. Time and cross-sectional averaged void fractions determined by the RTNR system agree within 4% with those determined by the high speed X-ray CT technique. (orig.).
A Real-Time Neutron Radiography (RTNR) system and a high speed X-ray Computed Tomography (X-CT) system are used to determine the flow regime, the instantaneous cross-sectional averaged void fraction, and the time averaged void fraction in a vertical annulus flow channel. A standard optical video system is also used to observe the flow regime. The annulus flow channel is operated as a bubble column and measurements are obtained for gas flow rates form 0.0 to 30.0 l/min. The flow regimes observed by all three measurement systems via image analysis shows that the results agree well with each other. Both the RTNR and the X-CT systems show that the time averaged and cross-sectional averaged void fraction increases with increasing superficial gas velocity. Time and cross-sectional averaged void fractions determined by the RTNR system agree within 4% with those determined by the high speed X-ray CT technique. (orig.).
We present the results of a search for Extreme Ultraviolet emission in A4059, a cluster with an X-ray emitting cluster gas. Our analysis of Extreme Ultraviolet Explorer (EUVE) Deep Survey observations of this cluster shows that it is associated with diffuse EUV emission. Outside the central 2 arcmin radius the entire EUV emission detected is explained by the low energy tail of the X-ray emitting gas. Within the central 2 arcmin region of the cluster we find a deficit of EUV emission compared to that expected from the X-ray gas. This flux deficit is discussed in the context of the cluster's cooling flow. The results derived for A4059 are compared to EUVE results obtained for other clusters such as Coma, Virgo, A1795, and A2199. As part of the study we have carried out a detailed investigation of the stability of the EUVE Deep Survey detector background. Based on long integrations of blank sky over 27 ...
The semiconducting compound CuGa_xIn_1_-_xSe_2 crystallizes in the chalcopyrite structure (space group Ianti 42d, Z=4). The X-ray powder data for x=1, 0.75, 0.6, 0.5, 0.4, 0.25 and 0.0 have been collected and it is found that the lattice parameters a and c and their ratio c/a vary linearly with x. Thus the composition of any chalcopyrite in the pseudo-binary system CuGaSe_2 and CuInSe_2 can be obtained from the accurate lattice parameters. The crystallite size determined from the (112) plane is minimum for x=0.50 (#propor to#1000 A) and away from x=0.50 it increases. A value of u=0.240 (5) has been established for fixing, the Se-atom positions in the CuGa_0_._5In_0_._5Se_2 solid solution. The JCPDS Diffraction File No. for CuInSe_2 is 40-1487 and for CuGa_0_._5In_0_._5Se_2 is 40-1488. (orig.).
Phase relations in the ternary system Ce-Pd-Si have been established for the isothermal section at 800degreeC based on X-ray powder diffraction and EMPA techniques on about 130 alloys, which were prepared by arc-melting under argon or powder reaction sintering. Eighteen ternary compounds have been observed to participate in the phase equilibria at 800degreeC. Atom order was determined by direct methods from X-ray single-crystal counter data for the crystal structures of t8-Ce3Pd4Si4 (U3Ni4Si4-type, Immm; a=0.41618(1), b=0.42640(1), c=2.45744(7)nm), t16-Ce2Pd14Si (own structure type, P4/nmm; a=0.88832(2), c=0.69600(2)nm) and also for t18-CePd1-xSix (x=0.07; FeB-type, Pnma; a=0.74422(5), b=0.45548(3), c=0.58569(4)nm). Rietveld refinements established the atom arrangement in the structures of...
For the first time, rheological phase method, a simple and effective route, is applied to synthesize novel cathode material LiCoPO{sub 4}. X-raydiffraction spectrometer (XRD), X-ray photoelectron spectrometer (XPS), transmission electron microscope (TEM) and electrochemical impedance spectroscopy (EIS) are taken to investigate this material, respectively. XRD figure shows that the rheological sample is better crystallized than the solid-state one. XPS result of the rheological sample exhibits that the valence of Co is 2+. TEM images show that better dispersed particles with smaller size can be formed by rheological method comparing to the solid-state route. Charge-discharge test is carried out in the range of 3.0-5.0 V at 0.2 mA cm{sup -2}. The initial discharge capacity for rheological phase and solid-state powder is 71.5 and 30.9 mAh g{sup -1}, respectively. The better electrochemical property should be ascribed to the ...
For the first time, rheological phase method, a simple and effective route, is applied to synthesize novel cathode material LiCoPO4. X-raydiffraction spectrometer (XRD), X-ray photoelectron spectrometer (XPS), transmission electron microscope (TEM) and electrochemical impedance spectroscopy (EIS) are taken to investigate this material, respectively. XRD figure shows that the rheological sample is better crystallized than the solid-state one. XPS result of the rheological sample exhibits that the valence of Co is 2+. TEM images show that better dispersed particles with smaller size can be formed by rheological method comparing to the solid-state route. Charge-discharge test is carried out in the range of 3.0-5.0 V at 0.2 mA cm-2. The initial discharge capacity for rheological phase and solid-state powder is 71.5 and 30.9 mAh g-1, respectively. The better electrochemical property should be ascribed to the better crystallized ...
Thermochromic tungsten-doped vanadium dioxide (VO2) powders were successfully synthesized by thermal reduction using V2O5 as a vanadium precursor. The products were characterized by X-raydiffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The results indicated that W was successfully doped into the crystal lattice of VO2 matrix, and prepared tungsten-doped VO2 had a rod-like morphology. The effects of reducing temperature and annealing temperature on the crystallographic structures were also discussed. The phase transition temperature (Tt) of VO2 could be simply tuned by changing the doping concentration of tungsten. When the doping concentration was 1.58 mol%, the Tt could be reduced to 37.8 oC from initial 69.5 oC, suggesting that tungsten-doped VO2 possesses prominent thermochromic properties and optical switching characters. It has ...
Herein, we report engineering of nanostructured p-CuIn3Se5/n-CdS heterojunction thin film on a glass substrate, which is prepared at room temperature using simple wet chemical approach involving ion exchange reactions between CdS and Cu^+, In^3^+ and Se^2^- ions in alkaline medium. The uniform deposition of heterojunction thin films is achieved by optimizing the pH, temperature and molarity of the reactant bath. The as-deposited thin-films were annealed at 200^oC in air for 1h and further characterized for structural, optical and electrical properties using UV-Vis spectrophotometer, X-raydiffraction (XRD), scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy (XPS), Hall effect for type of conductivity, and I-V measurement to investigate the char...
Ion bombardment during deposition can significantly modify the film properties. In the partially ionized beam deposition, ions derived from the depositing material, i.e., the self-ions, are used during deposition. Cu films were deposited on SiO_2 substrates at room temperature using 1% Cu self-ions with an energy ranging between 0--4 keV. We studied the microstructures of the Cu films using x-raydiffraction and transmission electron microscopy, measured the impurity level inside the films using secondary ion mass spectrometry, and performed the resistivity measurements using a four point probe. The results indicate that there is an optimum ion energy around 2 keV at which, the integrated x-ray intensity ratio I(111)/I(200) reaches its maximum value indicating a strong left-angle 111 right-angle texture, while the impurity concentration and resisitivity are minimum. The correlation between the structural, compositional and ...
Ion bombardment during deposition can significantly modify the film properties. In the partially ionized beam deposition, ions derived from the depositing material, i.e., the self-ions, are used during deposition. Cu films were deposited on SiO{sub 2} substrates at room temperature using 1% Cu self-ions with an energy ranging between 0--4 keV. We studied the microstructures of the Cu films using x-raydiffraction and transmission electron microscopy, measured the impurity level inside the films using secondary ion mass spectrometry, and performed the resistivity measurements using a four point probe. The results indicate that there is an optimum ion energy around 2 keV at which, the integrated x-ray intensity ratio {ital I}(111)/{ital I}(200) reaches its maximum value indicating a strong {l angle}111{r angle} texture, while the impurity concentration and resisitivity are minimum. The correlation between the structural, ...
Ion bombardment during deposition can significantly modify the film properties. In the partially ionized beam deposition, ions derived from the depositing material, i.e., the self-ions, are used during deposition. Cu films were deposited on SiO{sub 2} substrates at room temperature using 1% Cu self-ions with an energy ranging between 0--4 keV. We studied the microstructures of the Cu films using x-raydiffraction and transmission electron microscopy, measured the impurity level inside the films using secondary ion mass spectrometry, and performed the resistivity measurements using a four point probe. The results indicate that there is an optimum ion energy around 2 keV at which, the integrated x-ray intensity ratio {ital I}(111)/{ital I}(200) reaches its maximum value indicating a strong {l angle}111{r angle} texture, while the impurity concentration and resisitivity are minimum. The correlation between the structural, ...
Abstract Visible blue cathodoluminescence (CL), photoluminescence (PL), x-ray excited optical luminescence (XEOL) and electroluminescence (EL) via Zf free excitonic emission have been obtained from CuBr thin films deposited on glass, Cr coated glass, GaAs and Si substrates. In addition to the Zf emission several peaks corresponding to Cu+ emissions via 3d94s - d10 transitions were observed on the AC EL spectrum at 2.10, 2.7, 3.03, 3.07 and 3.80 eV. X-raydiffraction (XRD) measurements confirmed that the vacuum evaporated CuBr thin films grow preferentially with a (111) orientation irrespective of the substrate. While the AC voltage source was found to have no detrimental effects on CuBr thin films, cathodic deposition of Cu metal via electrolytic decomposition was observed under steady sta...
In this work we investigate an iron oxide thin film grown with atomic layer deposition for a gas sensor application. The objective is to characterize the structural, chemical, and electrical properties of the film, and to demonstrate its gas-sensitivity. The obtained scanning electron microscopy and atomic force microscopy results indicate that the film has a granular structure and that it has grown mainly on the glass substrate leaving the platinum electrodes uncovered. X-raydiffraction results show that iron oxide is in the #alpha#-Fe_2O_3 (hematite) phase. X-ray photoelectron spectra recorded at elevated temperature imply that the surface iron is mainly in the Fe"3"+ state and that oxygen has two chemical states: one corresponding to the lattice oxygen and the other to adsorbed oxygen species. Electric conductivity has an activation energy of 0.3-0.5 eV and almost Ohmic current-voltage dependency. When exposed to O_2 ...
We describe a panoramic stigmatic spectrograph comprising a grazing-incidence toroidal mirror and a large-aperture free-standing transmission diffraction grating (5000 lines mm-1 ). Two spectrograph versions were constructed, with grazing angles of 7.6 and 40 and the short-wavelength spectral limits near 4 and 1.5 nm. The spectrograph aberrations were studied by numerical ray tracing. The spectrograph was used to record line and quasi-continuous spectra (1.5 - 30 nm) of multiply charged ions in a plasma generated by the second-harmonic pulses of an yttrium aluminate laser (Q = 0.15 J, ? = 5 ns, ? = 0.54 ?m, repetition rate = 0.5 Hz). In combination with a laser-produced plasma radiation source, the arrangement was used to characterise soft x-ray optical components and to generate collimated beams of polarised radiation in the 14 - 20 nm range. (laser applications and other topics in quantum electronics)
Monodisperse europium-activated titania hollow phosphors had been synthesized by a facile one-pot hydrothermal method using carbon spheres as hard templates. Samples were characterized by X-ray powder diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, energy dispersive spectrometer and photoluminescence spectrum. The strongest emission intensity was observed with TiO2:Eu0.2 hollow spheres and TiO2:Eu0.2 hollow spheres calcining at 550^oC. Moreover, the strongest excitation of TiO2:Eu0.2 hollow spheres transferred from 400 to 500^oC and the effective nonradiative energy transfer from the TiO2 hollow spheres host matrix to Eu^3^+ ions crystal field states was realized due to changes of crystalline field in the environment around Eu^3^+ ions occupying Ti^4^+ site...
We propose and demonstrate a facile room-temperature synthetic method for obtaining water-soluble magnetic Fe3O4 nanoparticles (NPs) by combining the in situ synthesis and decomposition of a magnetic polymer hydrogel. The Fe3O4 NPs with average diameters of 6.3-8.3nm were synthesized in a cross-linked polyacrylamide (PAAm) hydrogel by coprecipitating iron ions. The decomposition of the magnetic polymer hydrogel by an aqueous solution of sodium hydroxide led to the transfer of Fe3O4 NPs into the aqueous medium. The NPs can be dispersed stably in water for more than three months. The Fe3O4 NPs were characterized by X-ray photoelectron spectra (XPS), X-ray powder diffraction (XRD), transmission electron microscope (TEM), and Fourier transform infrared spectroscopy (FT-IR). The saturation magn...
Results of X-ray investigations of solid normal hydrogen are presented. Temperature dependences of the lattice parameteps, molar volumes, linear and volume expansion coefficients in the 2K-Tsub(melt) temperature range are obtaiped. An essential n-H/sub 2/ expansion anisotropy in the premelting temperature region is pointed out. It is shown that the hexagonal lattice parameter ratios over the whole investigated temperature range is considerably higher than for solid parahydrogen. A considerable difference in thermal expansion of normal hydrogen and parahydrogen in the low temperature region is revealed. It is caused by contribuation of a rotational subsystem, increasing with the temperature decrease to crystal expansion. A detailed analysis of solid n-H/sub 2/ thermodynamic properties is conducted. The data testifying to the presence of isomorphous phase transformation in the solid n-H/sub 2/ in the premelting temperature region are discussed.
Radionuclide X-ray fluorescence analysis (RXRFA), as a non-destructive method, relatively simple and allowing measurements to be carried out in situ, is an excellent tool in research on various objects of art. A range of artefacts have been investigated by our laboratory, in part for the purposes of history of art and in part as a basis for restoration works - medieval frescoes in some Czech castles and churches, metal sculptures and objects of applied art, paints and inks of old manuscripts, paintings. Some of these are among the most valuable monuments in the Czech cultural heritage. The contribution of the results of the tests to the investigation of their 'life story' and, in some cases, to their conservation, is not negligible. Later additions and repairs can be recognised, and materials and technologies that are close to their historic counterparts can be used in restoration work.
Radionuclide X-ray fluorescence analysis (RXRFA), as a non-destructive method, relatively simple and allowing measurements to be carried out in situ, is an excellent tool in research on various objects of art. A range of artefacts have been investigated by our laboratory, in part for the purposes of history of art and in part as a basis for restoration works - medieval frescoes in some Czech castles and churches, metal sculptures and objects of applied art, paints and inks of old manuscripts, paintings. Some of these are among the most valuable monuments in the Czech cultural heritage. The contribution of the results of the tests to the investigation of their 'life story' and, in some cases, to their conservation, is not negligible. Later additions and repairs can be recognised, and materials and technologies that are close to their historic counterparts can be used in restoration work.
Radiation damage is considered to be the major problem that still prevents imaging an individual biological molecule for structural analysis. So far, all known mapping techniques using sufficient short wave-length radiation, be it X-rays or high energy electrons, circumvent this problem by averaging over many molecules. Averaging, however, leaves conformational details uncovered. Even the anticipated use of ultra-short but extremely bright X-ray bursts of a Free Electron Laser shall afford averaging over 10^6 molecules to arrive at atomic resolution. Here we present direct experimental evidence for non-destructive imaging of individual DNA molecules. In fact, we show that DNA withstands coherent low energy electron radiation with deBroglie wavelength in the Angstrom regime despite a vast dose of 10^8 electrons/nm^2 accumulated over more than one hour.
As to all sinter variations the microradiographic analysis showed that about 86 to 90 % of the implant surface were enclosed split-free with newly formed bone 16 weeks post operationem. A silicat salt addition of the test variation Ap_4_0KS_1_5 and Ap_4_0KS_3_0 did not cause a negative influence on bone regeneration. On the surface of all test implants a double layer was revealed radiologically, consisting of a 30 - 40 #mu#m thick bone near X-ray impermeable area and an X-ray permeable area of maximum 120 #mu#m thickness directed to the nucleus of the implant.
As to all sinter variations the microradiographic analysis showed that about 86 to 90 % of the implant surface were enclosed split-free with newly formed bone 16 weeks post operation. A silicate salt addition of the test variation Ap/sub 40/KS/sub 15/ and Ap/sub 40/KS/sub 30/ did not cause a negative influence on bone regeneration. On the surface of all test implants a double layer was revealed radiologically, consisting of a 30 - 40 ..mu..m thick bone near X-ray impermeable area and an X-ray permeable area of maximum 120 ..mu..m thickness directed to the nucleus of the implant.
The radionuclide X-ray fluorescence analyzer consists of a source changer and a sample changer. "5"5Fe, "1"0"9Cd and "2"4"1Am are used as excitation sources. The radiation is detected with a semiconductor Si(Li) detector. The complete assembly of the apparatus consists of an imagine unit, a keyboard, a floppy disc drive, a printer, a console and a rack with analog and digital electronics. Its multichannel amplitude analyzer consists of power supplies, a high voltage supply, a linear amplifier, an analog-to-digital converter and a computer. The technical specifications are given. The control and data processing system is controlled with an MHB 8080A microprocessor. Software for semiconductor gamma spectrometry and for quantitative gamma spectrometry will be supplied with the equipment. (E.S.). 3 figs., 4 refs.
A micropositioning stage for use with an x-ray microscope has been developed to scan samples over a 100 {mu}m{times}100-{mu}m area with a resolution of 100 A. The stage employs flexure hinges driven by piezoelectric actuators to achieve this high positioning accuracy. Due to the severe geometry of the hinges, stresses and deflections are determined (via finite element methods) to ensure a credible design. Since the stage is to be used in a stepping capacity, natural frequencies are computed to identify resonant conditions which could potentially cause excessive deflections. The finite element models show that the stage responds like a discrete lumped-mass system for the lower modes, and a continuous system with flexural characteristics for the higher modes.
An iterative phase retrieval algorithm was previously investigated for in-line x-ray phase imaging. Through detailed theoretical analysis and computer simulations, we now discuss the limitations, robustness, and efficiency of the algorithm. The iterative algorithm was proved robust against imaging noise but sensitive to the variations of several system parameters. It is also efficient in terms of calculation time. It was shown that the algorithm can be applied to phase retrieval based on one phase-contrast image and one attenuation image, or two phase-contrast images; in both cases, the two images can be obtained either by one detector in two exposures, or by two detectors in only one exposure as in the dual-detector scheme.
Cluster calculations of the electronic structure and charge distribution in V_3Si have been performed using two different molecular orbital methods: a semiempirical LCAO and the MS X#alpha# model. The results are compared with X-ray emission spectra and band structure calculations. An analysis of the calculated electronic distribution reveals a charge transfer from Si-atoms to V-atoms, the additional charge on a V-atom being 0.6e (LCAO) and 0.4e (MS X#alpha# method). The results are in good agreement with experiment, which indicates that the cluster approach is adequate for the description of charge distributions and spectra characteristics of the A-15 compounds. (author).
We present constraints on theoretical models of Type Ia SNe using spatially resolved ASCA X-ray spectroscopy of four galaxy clusters: Abell 496, Abell 2199, Abell 3571 & Perseus. All four clusters have central Fe abundance enhancements and an ensemble of abundance ratios are used to show that most of the Fe in the central regions of the clusters comes from SN Ia. At the center of each cluster, simultaneous analysis of spectra from all ASCA instruments shows that the Ni to Fe abundance ratio (normalized by the solar ratio) is ~ 4. We use the Ni/Fe ratio as a discriminator between SN Ia explosion models: the Ni/Fe ratio of ejecta from the "Convective Deflagration" model W7 is consistent with the observations, while those of "delayed detonation" models are not consistent at the 90% confidence level.
Fuji Computed Radiography (FCR) is a new system of digital radiography that is based on the latest computer technologies. We applied this FCR system to the X-ray diagnosis of the laryngeal disease. Twenty patients with various laryngeal diseases were evaluated by both FCR frontal tomography and conventional screen-film frontal tomography under the same exposure condition. Both tomograms were then compared on the subject of the clarity of delineation of laryngeal structures. As the result, FCR tomograms revealed the feature of the laryngeal lumen and cartilages more clearly than conventional tomograms. In addition, energy subtraction method, which is one of FCR image processing systems, was presented as a new technical procedure to extinguish cervical spine shadows in plain anteroposterior laryngeal X-photograph. We stress that FCR system is the suitable procedure for X-rayanalysis of laryngeal diseases, especially in the ...
Fuel cells based on solid oxides ('SOFC') are excellent alternative devices for power generation, when they are operated at high temperature, e.g. above 600 C. Having only fixed parts for the power generating part of the device is only one advantage of the fuel cell. Due to their unique design, these devices offer a maximum of efficiency for energy conversion compared to conventional power generating systems, which are mainly based on turbines. One aim of this thesis is the examination of alternative electrolyte and cathode materials for the SOFC applications at reduced temperatures, which means in the temperature range between 600 C and 750 C. For the first main task, several materials from the oxygen ion conducting electrolytes were selected. Different strontium and magnesium doped lanthanum gallate (LSGM) materials with additional transition metal doping were selected and prepared via two different preparation methods. The optimum calcining conditions were ...
The standard deviation of measurement results of a given element in XRF spectrometry depends on three factors: concentration and concentration region, atomic number and matrix. The effects of these factors were investigated by an XRF instrument type ARL 72.000 for aluminium metal, bauxite-red mud and aluminium using computerized data processing. A comparison of linear and nonlinear relation between concentration and the result of XRF analysis was made for the determination of standard deviation. (R.P.).
Determination of Cr, Fe, Cu, Zn and Pb in drinking water preconcentrated on a chelating ion exchanger of Czechoslovak production is described. The analytical system consisted of a radionuclide source "2"3"8Pu, a Si/Li semiconductor detector and a multichannel analyzer. Results are compared with trehshold limit values recommended for drinking water. (author) 9 refs.; 2 figs.
Plantago ovata Forsk - an economically important medicinal plant - was analyzed for trace elements and chlorophyll in a study of the effects of gamma radiation on physiological responses of the seedlings. Proton-induced X-ray emission (PIXE) technique was used to quantify trace elements in unirradiated and gamma-irradiated plants at the seedling stage. The experiments revealed radiation-induced changes in the trace element and chlorophyll concentrations.
In the present paper the progress of optimization of soft magnetic properties have been studied by applying different experimental techniques (magnetic measurements, electric measurements, X-rayanalysis, and high-resolution electron microscopy observation). It has been shown that an increase in magnetic permeability after optimization annealing can be mainly attributed to annealing out of microvoids. (author)
From the frequency of diagnostic radiologic examinations and their radiation dose delivered to the population the risk of cancer induction and genetic damage is calculated on the basis of the risk factors given by the ICRP. Thus 0.38 % and 3 % of the total mortality for cancer and leukemia, resp., can be attributed to X-ray diagnostics. Chest examinations alone result in 0.07-0.7 damages per 100,000 persons depending on the imaging technique applied. (author).
The etching method developed made it possible to observe under the microscope the finest components of the anatomical structure of coal-forming plants. The dependence of the effectiveness of etching of tissues on the concentrations of geopolymers (protocellulose and protolignin) in them was found. The study of tissues of this kind by the methods of local analysis (for example, X-ray microanalysis) allowed us to obtain the characteristics of the above geopolymers and to use them for the identification of the primary biochemical composition of fossil organic matter.
Elements Ti, Mn, Fe, Ni, Cu, Zn, Pb, Br, Rb and Sr were determined by the method of radionuclide X-ray fluorescence analysis with semiconductor detection in samples of Taraxacum officinale from various localities of Bratislava. The dependence of their content on the source and the degree of the air pollution was found out.
Elements Ti, Mn, Fe, Ni, Cu, Zn, Pb, Br, Rb and Sr were determined by the method of radionuclide X-ray fluorescence analysis with semiconductor detection in samples of Taraxacum officinale from various localities of Bratislava. The dependence of their content on the source and the degree of the air pollution was found out. (author).
Fe, Mn, Ni, V, Ti and Mo were determined in aerosols from manual arc welding. Samples of welding aerosols were trapped on a Synpor 4 filter. The amount of determined elements in aerosols was detected using the method of radionuclide X-ray fluorescence analysis. A /sup 241/Am annular source was used as the source of excitation radiation and radiation was processed using a Si(Li) spectrometer.
Fe, Mn, Ni, V, Ti and Mo were determined in aerosols from manual arc welding. Samples of welding aerosols were trapped on a Synpor 4 filter. The amount of determined elements in aerosols was detected using the method of radionuclide X-ray fluorescence analysis. A "2"4"1Am annular source was used as the source of excitation radiation and radiation was processed using a Si(Li) spectrometer. (E.S.).
We determined the Na/K x-ray intensity ratio in frozen sections of myocardial tissues obtained at autopsy from patients who died from various causes, using electron probe analysis. We have been able to distinguish between the ischemically injured and normal cells. The method is simple, fast, and dependable even when the duration of ischemia is only 30 minutes.
Radionuclide X-ray fluorescence analysis was used for the determination of Sr/Ca ratio in bones to test the influence of a diet on this ratio. Significant differences were observed for Sr/Ca ratio in bones of various animals. Only small differences in the Ca/Sr ratio were observed for the samples of various prehistoric human bones. (author) 4 refs.; 4 tabs.
Trace elements have been determined in biological samples including pepperwort, thyme, plantain, blessed thistle and common comfrey as well as cabbage leaves and milk powder. Concentrations of Al, Si, and Cl have been determined by fast neutron activation analysis while, in the case of Mg-, K, and Cl the X-ray fluorescence method was used.
All organisms examined to date possess a dUTPase that performs the important function of efficiently hydrolyzing dUTP to dUMP in order to prevent the incorporation of dUTP into DNA. Three putative dUTPases...Full Text Available
A computerised curve-fitting method was developed to calculate the trapping parameters in LiF TLD-100 and LiF:Mg, Ti. After irradiation in a "6"0Co field and with Xrays emitted at different voltages the TL process is best described by first-order kinetics. A dependence of the trapping parameters on both the concentration of Mg and Ti and photon energy was detected. (author).
The first step in the protection of the environment is the control of pollutant level in the components of the environment. The application is compared of radionuclide X-ray fluorescence analysis (RXFA) used for this purpose with polarographic and nuclear analytical techniques. The advantage of RXFA is its high sensitivity and selectivity, its low time and cost exactingness. The origins and development of RXFA are described. (Ha).
Doping of manganese (Mn3+/Mn4+) into the Aurivillius phase Pb1-xBi4+xTi4-xMnxO15 was carried out using the molten salt technique for various Mn concentrations (x=0, 0.2, 0.4, 0.6, 0.8, and 1). Single phase samples could be obtained in the composition range with x up to 0.6 as confirmed by X-ray and neutron diffractionanalysis. Dielectric measurements show a peak at 801, 803, 813 and 850 K for samples with x=0, 0.2, 0.4, and 0.6, respectively, related to the ferroelectric transition temperature (Tc). The main contribution of the in-plane polarization for x?0.2 which was calculated from the atomic positions obtained by the structure analysis is the dipole moment in the Ti(1)O6 layer; however, for x?0.4 the polarization originates from the dipole moment in the Ti(2)O6 layer. Mn doping in the Pb1-xBi4+xTi4-xMnxO15 does not show any long range magnetic ordering. -- Graphical abstract: The dipole moment of ...
The purpose of this work is to present a comprehensive, instructive analysis of the basis of radionuclide XRFA, to describe methods of sample preparation for environmental analysis and to make the reader more familiar with the procedures, methods and instrumentation of radionuclide XRFA used in this field. This book discusses the use of radionuclide XRFA for solving analytical problems of the environment and information is presented concerning the current state of research and use of radionuclide XRFA in this significant area. The present volume will serve as a basic source of data and also as a laboratory handbook. refs.; figs.; tabs.
Characterization of high temperature superconducting film and bulk samples has been carried out using 2 MeV [alpha]-particle Rutherford backscattering, 2.4 MeV proton elastic scattering, 2.4 MeV proton-induced x-ray emission, 9 MeV proton induced [gamma]-ray emission and 100 MeV iodine elastic recoil detection analysis techniques. The objective was to compare different ion beam based techniques for: (i) compositional analysis; and (ii) consistency of the results obtained for samples prepared using similar preparation methodology. (author).
Instrumental neutron activation analysis (INAA) and radionuclide X-ray fluorescence analysis (RXFA) were used for the determination of rare earth elements. For INAA, solution obtained by sample decomposition was dripped onto filter paper, enclosed and sealed into a polyethylene foil. The sample was activated in reactor WWR-S over a period of 4 to 6 hours with a neutron fluence of 10"1"3cm"-"2. Gamma radiation measurement was carried out with a planar and a coaxial HP-Ge detector in three decay periods. La, Ce, Nd, Sm, Eu, Gd, Tb, Ho, Tm, Yb and Lu were determined. The advantage of the method is its accuracy and high sensitivity, the disadvantage is the time-consuming analysis. The RXFA method was used as a rapid and operative method for the analysis of loose ore samples, aqueous and organic solutions of rare earth elements. For exciting X-ray radiation, "2"4"1Am ...
Circularly polarized X-rays produced by a diamond X-ray phase retarder of thickness 0.5 mm in the Laue transmission configuration have been used for recording X-ray magnetic circular dichroism...Full Text Available
Fe-doped TiO2 hollow spheres (Fe-THs) were synthesized by sol?gel process using carbon spheres as templates. The prepared samples were characterized by X-raydiffraction (XRD), transmission electron microscopy (TEM), UV?vis diffuse reflectance spectrum (DRS), N2 adsorption?desorption isotherms, Electron paramagnetic resonance (EPR) spectroscopy and Photoluminescence emission spectroscopy (PL). UV?vis spectra showed that Fe3+ doping could extend the absorption edge to the visible region. EPR spectra showed that Fe3+ was incorporated into the crystal lattice of TiO2, which could inhibit the recombination of photo-induced electron?hole pairs and improve the photocatalytic activity. The photocatalytic activities of the prepared samples were evaluated for the degradation of dye Reactive Brillia...
The TiO2 hollow microspheres were prepared by microwave-assisted solvothermal treatment without template. The morphology and the phase of TiO2 hollow microspheres were characterized by X-raydiffraction (XRD), field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HR-TEM), and BET surface areas. The results show that the particles have hollow structures and the shell was covered by nanocrystals and have higher specific surface area. The possible formation mechanism of hollow TiO2 spherical structures has simply been proposed. The activity was evaluated by the photocatalytic degradation of methyl orange (MO). The results show that the particles having specific surface area show higher photocatalytic activity. It can be attribute to the doped ...
In this paper, the influence of plasma nitriding at temperature 720 deg. C for 20 h on the surface microstructure and interface microstructure of electroplated chromium coating was investigated. In these conditions, interdiffusion, mixing and reaction phenomena of elements originating from the substrate and coating material are more likely to occur, thus increasing the bonding strength between the coating and carbon steel substrate. The change of the structures from the substrate side to the coating surface, and the effect of the substrate steel on the interface structure were studied by cross-sectional transmission electron microscope observation (XTEM). The nitride layer formed on the surface was analyzed by X-raydiffraction method (XRD). After treatment at above conditions a 6-7 {mu}m thick nitride compound layer was formed in surface region and the same thick carbide compound layer was also formed in the interface region between ...
In this paper, the influence of plasma nitriding at temperature 720 deg. C for 20 h on the surface microstructure and interface microstructure of electroplated chromium coating was investigated. In these conditions, interdiffusion, mixing and reaction phenomena of elements originating from the substrate and coating material are more likely to occur, thus increasing the bonding strength between the coating and carbon steel substrate. The change of the structures from the substrate side to the coating surface, and the effect of the substrate steel on the interface structure were studied by cross-sectional transmission electron microscope observation (XTEM). The nitride layer formed on the surface was analyzed by X-raydiffraction method (XRD). After treatment at above conditions a 6-7 #mu#m thick nitride compound layer was formed in surface region and the same thick carbide compound layer was also formed in the interface region between ...
The thermal stability of nanoscale grains in cryomilled aluminum powders containing 1% diamantane was investigated. Diamantane is a diamondoid molecule consisting of 14 carbon atoms in a diamond cubic structure that is terminated by hydrogen atoms. The nanostructures of the resulting cryomilled powders were characterized using both transmission electron microscopy (TEM) and X-raydiffraction (XRD) techniques. The average grain size was found to be on the order of 22?nm, a value similar to that obtained for cryomilled Al without diamantane. To determine thermal stability, the powders were heated in an inert gas atmosphere at constant temperatures between 423 and 773?K (0.51T m to 0.83T m) for exposure times of up to 10?h. The average grain size for all powders containing diamantane was obse...
In this study polycrystalline specimens of as-cast DyCu with B2 crystal structure were compressed to different strains at room temperature to test if stress-induced phase transformation and twinning occur during deformation. In these tests DyCu exhibited high ductility with plastic strain as high as 35% and ultimate compressive strength of ~790MPa. X-raydiffraction and transmission electron microscopy (TEM) showed no indications that DyCu had undergone stress-induced phase transformation or twinning. -type dislocations have been observed to play an important role for imparting the ductile behavior. TEM analyses showed the presence of second phases, Dy2O3 and DyCu2 within the DyCu. The mechanisms of ductility and impurity phase formation are discussed.
Antibacterial activity of Transition metals (Mn, Co) doped ZnO nanopowders prepared by a DC thermal plasma method against Escherichia coli and Staphylococcus aureus are investigated. The phase and morphology studies have been carried out by X-raydiffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. All the samples of the present investigation are found to have hexagonal wurtzite structure and crystallite sizes are found to vary from 25nm to 30nm. Our bacteriological study showed the enhanced antibacterial activity of transition metals doped ZnO nanoparticles than undoped ZnO indicating the great potential of ZnO nanoparticles in relevant clinical and biomedical applications.
In this article, we describe a method used to prepare an in situ sodium-activated, organomodified bentonite clay/styrene-butadiene rubber nanocomposite master batch via a latex blending technique. The clay master batch was used for compound formulation. Octadecyl amine was used as an organic intercalate. The clay was purchased from local suppliers and was very cheap. Sodium chloride was used for in situ activation of the clay. The wide-angle X-raydiffraction data indicated that the in situ sodium activation helped to increase the intergallery distance from 1.28 to 1.88 nm. A transmission electron micrograph indicated intercalation and partial exfoliation. The thermal properties were relatively better in the case of the sodium-activated, organomodified bentonite-clay-containing compound. A...
We synthesized Fe3O4Gg nanocomposites through a combination of solvothermal, hydrothermal, and chemical redox reactions. Characterization of the resulting samples by X-raydiffraction, Fourier-transform infrared spectroscopy, field-emission scanning and transmission electron microscopy, and magnetic measurement is reported. Compared to Fe3O4g nanocomposites, the Fe3O4Gg nanocomposites showed enhanced antibacterial activity. The Fe3O4Gg nanocomposites were able to almost entirely prevent growth of Escherichia coli when the concentration of Ag nanoparticles was 10mg/mL. Antibacterial activity of the Fe3O4Gg nanocomposites was maintained for more than 40h at 37^oC. The intermediate carbon layer not only protects magnetic core, but also improves the dispersion and antibacterial activity of the...
Bilayers of pure palladium and gold films were evaporated alternatively on (100) and (111) monocrystalline silicon substrates. After annealing, in a vacuum furnace from 100 to 650degreeC during 30min, the growth sequence of the Pd2Si and PdSi phases that evolved as the result of the diffusion reaction was examined by means of Rutherford backscattering spectrometry (RBS), X-raydiffraction (XRD), whereas the surface morphology was investigated by scanning electron microscopy (SEM) technique. The effect of the intermediate gold layer is investigated in order to test its effectiveness as barrier for Cu and Si atoms interdiffusion and its influence on the morphology of the formed palladium silicides. The effect of substrate orientation on the palladium silicides growth and formation was also e...
Nuclear forensic activities, such as in illicit trafficking, can solve a problem who did it and can gain the basis for a response. Other than that, the forensics can be also applied to solve on what are materials, who is responsible, is there more, where was material diverted and what route did the material taken. BATAN, in fact , owns a lot of equipment which can be supported for nuclear forensics activities, such as, Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM) as well as X-RayDiffraction (XRD). For the first step, BATAN has to be an active, participate member of The International Technical Working Group on Nuclear Smuggling (ITWG). BATAN can then collaborate not only with Indonesia Arm Forces and Police, but also with other foreign institutions to develop this activity with mutual advantages agreement.
Three-dimensional porous Sn thin film electrodes were prepared by electroless deposition on copper foam, then its morphology and electrochemical property were studied by means of scanning electron microscope (SEM), X-raydiffraction (XRD), electrochemical cycling test and cyclic voltammetry (CV). The porous framework and micro-holes have shown a great structure advantage in restricting severe volume changes when the Sn thin film was employed as anode for lithium-ion battery. The film electrode of sample C with an initial capacity of 676 mAh g{sup -1} showed good cycle performance displayed by retaining a capacity of 313 mAh g{sup -1} after 100 cycles.
The constituent phases and associated deformed microstructure of the quenched Ti-xNb-(0.5-1.5) at.% Si alloy consisting of non-cytotoxicity elements, where x = 24-30 at.%, were investigated to provide pseudoelasticity for biomedical and sensor applications. Optical microscopy revealed that stress-induced martensitic transformation takes place during the deformation in the present alloys. It is confirmed from the X-raydiffraction results of the deformed specimens that the crystal structure of the stress-induced martensite phase is the orthorhombic so-called #alpha#'' structure. Within the alloys having #beta#(bcc) phase studied Nb-poor region appeared to exhibit a dominant behavior for stress-induced martensitic transformation than Nb-rich region. This result suggests that metastable #beta# phase is superior to stable #beta# phase for the occurrence of stress-induced martensitic transformation in the present alloy system.
Soluble starch?based biodegradable and microporous microspheres (SDM-Ms) were prepared by emulsion chemical cross-linking technique using trisodium trimetaphosphate (TSTP) as the cross-linker. The resultant amorphous SDM-Ms were excellently identified by scanning electron microscopy (SEM), X-raydiffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The internal rupture and surface-controlled erosion were the predominant degradation mechanisms for SDM-Ms. The obtained SDM-Ms were applied to adsorb coix seed oil (CSO) by immersing method. The adsorption capacity of CSO within SDM-Ms was determined, namely 0.5238?g/g, and the thermal stability was shown higher than that of the free CSO. A burst release appeared in the second hour, followed by controlled release. Diffusion, d...
Ag nanoparticles were prepared in a water-phase system with a mixture of silver-ammonia complex, sodium borohydride, and lauric acid according to molar feed ratio of approximately 6:3:1. The mechanism of preparation and separation by chemical reduction-protection method was explored. The as-synthesized Ag nanoparticles were characterized by transmission electron microscopy (TEM), X-raydiffraction (XRD) and UV-vis spectroscopy, respectively. It was found that the size of high purity Ag particles was ranging from 30 to 50 nm with slight agglomeration. In addition, the as-synthesized wet Ag nanoparticles were dispersed stably in organic vehicle to formulate electrically conductive nanopaste. Upon direct-written and sintered, the array pattern of the nanopaste with the resolution of about 30 {mu}m was achieved with the electrical resistivity in the order of magnitude of 10{sup -5} {Omega} cm.
The conductive ultra thin films were fabricated from mixed monolayers containing stearic acid and Head-to-Tail poly(3-alkylthiophene). These films exhibited well-defined layered structures as determined by optical absorption and X-raydiffraction measurements. The UV-Vis absorption spectra of these films showed lower energy absorption shifts of 48 nm from that of the random poly(3-alkylthiophene)/stearic acid LB films. The blue shift of absorption maximum of the LB film is attributed to the increase of {pi}-conjugation length caused by no steric hindrance of alkyl side chains. The conductivity of the Head-to-Tail poly(3-hexylthiophene)/stearic acid LB films was greatly improved in the range of 67-100 S/cm. (orig.)
Membranes in Palladium and its alloys, in particular Pd/Ag alloys, are selectively permeable to hydrogen and can therefore be used to purify hydrogen. It is intended to use them as material for electrodes in fuel cells. As the manufacturing process of a substrate Pd/Ag-layer consists of several stages and is still not completely understood, it would be advantageous to be able to characterise separately the layers of noble metals obtained by electro-plating . Attempts are being made in this work to vary the cristallographical structure of the deposited alloy by the choice of test parameters and by sintering when depositing the Pd/Ag. The layers produced are to be examined using an interference microscope and X-raydiffraction. Moreover, the diffusion behaviour of the hydrogen is to be examined with an electro-chemical pulse method specifically developed for this purpose. figs., tabs., 27 refs.
The noncrystalline compounds MoS_3, WS_3 and MoSe_3 were studied by X-raydiffraction. From the diffuse intensities radial distribution functions were computed and interpreted in terms of pair distribution functions. The substances are built up by microcrystallites which contain three metal atoms and are bridged statistically to each another. The shortest metal chalcogen distances d(MoS) approximately d(WS) = 2.40 +- 0.05 A and d(MoSe) = 2.50 +- 0.05 A are significantly longer than in MS- or MSe compounds with a d"0 configuration of the metal respectively and metal-metal distances within the microcrystallites are less than 3 A. (author).
The growth of silver chloride nanoparticles on ancient textile was achieved by sequential dipping steps in alternating bath of potassium chloride and silver nitrate under ultrasound irradiation. The effect of ultrasound irradiation and sequential dipping steps in growth of the AgCl nanoparticles has been studied. These systems depicted a decrease in the particles size accompanying a decrease in the sequential dipping steps. The samples were characterized with powder X-raydiffraction (XRD) and scanning electron microscopy. XRD analyses indicated that the prepared AgCl nanoparticles on fiber were crystalline. The textile samples containing AgCl nanoparticles were tested for their antibacterial efficacy against Escherichia coli and were found to possess significant antibacterial activity.
Microalloyed or high strength low alloy (HSLA) steels are carbon-manganese steels containing small amounts of Nb, V or Ti. The excellent mechanical properties of these alloys, particularly high yield strength, usually obviate the need for expensive quench and tempering operations. Furthermore, the presence of a significant amount of nitride-forming elements in some microalloyed steels has generated interest in the applicability of these alloys as a new generation of nitriding steels. In this paper, a study of the plasma nitriding behaviour of a commercially available microalloyed steel MAXIMA{sup TM} is reported. A comparison is made with a traditional quenched and tempered nitriding steel (En19), plasma nitrided under similar conditions. Optical and scanning electron microscopy in conjunction with microhardness measurements and X-raydiffraction were utilized to characterize the nitrided surfaces. The observed differences in the thickness and ...
In connection with the different cyclical strengths of the two-phase (#alpha# + #beta#) titanium alloy in the case of the acicular and rounded formations of the #alpha#-phase, we have studied, employing the X-raydiffraction method, the phase composition of the alloy and the influence of heat treatment upon it. Using the method of electronic fractography, we examined the fractures in samples destroyed by the asymmetric twisting, in order to find out why the durability of the alloy is dependent upon the #alpha# - phase structure. It has been found that in the BT22 alloy, the decay the #beta#-phase may proceed in two ways; either with the formation of the martensite #alpha#'-phase of the acicular shape or with the separation of the non-martensite round-shaped #alpha#-phase. The character of the phase transformations #beta# - #alpha# or #beta#-#alpha#' is, to a considerable extent, the conseguence of the prehystory of the alloy and is dependent ...
We present a synchrotron x-raydiffraction study of melting in stacks of two-dimensional crystalline arrays of the membrane protein bacteriorhodopsin. Two distinct regimes have been found as a function of the intermembrane distance d . In the {open_quotes}coupled{close_quotes} regime for d{lt}250 {Angstrom} the temperature (T{sub m}) of the melting transition decreases with increasing d , demonstrating the effect of the repulsive membrane interactions on the intramembrane protein ordering. For d{gt}250 {Angstrom} a {open_quotes}decoupled{close_quotes} regime is found with higher T{sup *}{sub m} independent of d . Below T{sup *}{sub m} a solid-liquid-solid reentrant behavior is observed as d is increased. {copyright} {ital 1999} {ital The American Physical Society}
Thin passive layers of uranium nitride were formed by nitriding pure metallic uranium in non-equilibrium, low pressure radio-frequency plasma of nitrogen. Plasma nitriding at low substrate temperature of 230 C-250 C was found to cause the formation of adherent layers of uranium sesquinitride ({alpha}-U{sub 2}N{sub 3}) which provide a considerable protection against hydrogen attack. The characteristics of these passivation layers were determined by X-raydiffraction and Auger electron spectroscopy. The incipient hydriding kinetics of the plasma-treated samples were compared with those of untreated and nitrogen-ion implantation ones, utilizing a hot-stage microscope that was monitored continuously with a TV camera and videotape. (orig.)
Copper complexes of the amino acids histidine, arginine and lysine have been introduced into the supercages of zeolite Y and, for the first time, into the large intracrystalline cavities of zeolites EMT and MCM-22. The resulting host/guest compounds are characterized by X-ray powder diffraction, UV/VIS-spectroscopy in the diffuse reflectance mode and by catalytic tests in the liquid-phase oxidation of aromatic alcohols (viz. benzyl alcohol, 2- and 3-methylbenzyl alcohol and 2,5-dimethylbenzyl alcohol) with tertiary-butylhydroperoxide as oxidant. It was observed that intracrystalline copper-amino acid complexes possess remarkable catalytic activity, yielding the corresponding aromatic aldehydes and acids. (orig.)
With the aim of optimizing the nitriding process, experimental studies of the plasma nitriding of four selected steels were carried out, using a d.c. glow discharge. The process parameters were varied systematically. By means of transmission and scanning electron microscopy and X-raydiffraction, the microstructures, including the thicknesses of the compound zones and the diffusion zones of the nitrided steels, were obtained. Using cross-sectional samples and a micro-Vickers indenter, hardness depth profiles were also obtained. From the time and temperature dependences of the hardness profiles, effective diffusion constants and corresponding activation enthalpies were obtained. Furthermore, in an attempt to shed some light on the atomistic nitriding mechanisms, the glow discharges were studied by measuring energy spectra of the energetic ions hitting the cathode (the steel test specimens). It was shown that an increase of the mean energy of the ...
Transmission electron microscopy and x-raydiffraction data show that rapid thermal anneals of SrS:Ce thin films enhance grain size and reduce crystalline defects. Electron paramagnetic resonance results suggest that these anneals lead to less variance in the crystal field environments at the nearly cubic Ce"3"+ sites along with the formation of another type of Ce"3"+ site believed to involve a nearby Sr vacancy. We suggest that the association of Ce"3"+ sites with V_S_r shifts the electroluminescence towards larger wavelengths as the symmetry of the activator site is lowered. copyright 1997 American Institute of Physics.
The microstructure of the layers produced by plasma nitriding austenitic stainless steel at different treatment temperatures (400 and 500 C) were studied by transmission electron microscopy (TEM) together with X-raydiffraction (XRD) and scanning electron microscopy (SEM). The results show that the microstructures were composed of 'expanded austenite' ({gamma}{sub N}) and {alpha}(ferrite)+CrN following plasma nitriding at lower and higher treatment temperatures, respectively. The former contains stacking faults and deformed twin substructures, while the latter is made up of colonies displaying a lamellar structure. Kurdjumov-Sachs or Nishiyama-Wassermann orientation relationships between the {alpha} and CrN layer were observed. (orig.)
Laser welding of AISI 904 L super austenitic stainless steel using a diffusion cooled slab 3.5kW CO2 laser and employing two different shielding gases, namely argon and helium, was carried out. The laser weld bead profile depends on various parameters such as beam power (BP), travel speed (TS) and focal position (FP) of the laser spot. These parameters have to be selected suitably to obtain the desirable output. The cross sectioned area of the bead profiles measured using an optical microscope to determine the bead width and depth of penetration. X-raydiffraction used for phase identification confirmed that the weld structure was fully austenitic and dendritic. Hardness was observed to increase in the weld bead with respect to the parent metal and it was related to the microstructural ref...
Regularities of deformation-induced dissolution of a surface layer of iron oxides in matrixes of iron-based alloys with bcc and fcc lattices have been studied by the methods of M?ssbauer spectroscopy, transmission electron microscopy, and X-raydiffraction. A method of producing iron alloys strengthened by dispersed oxide nanoparticles and alloyed with elements possessing a high affinity to oxygen (titanium and yttrium) has been proposed, which implies a dynamic dissolution of a surface layer of iron oxides upon strong cold deformation and a precipitation of secondary yttrium and titanium nanooxides upon a subsequent high-temperature sintering of mechanically alloyed powders. There has been demonstrated a possibility of oxide strengthening of pure iron upon its interaction with air without...
Cold spray was employed as a novel low temperature approach to deposit titanium dioxide (TiO{sub 2}) photocatalytic film. The film microstructure was characterized using X-raydiffraction and scanning electron microscopy. The photocatalytic performance was examined through acetaldehyde degradation under ultraviolet illumination. Results showed that TiO{sub 2} film was successfully deposited on substrate surface through cold spray. The film thickness reached up to 15 {mu}m. The film presented a rough surface and porous structure. Owing to the low temperature of spray powder, no phase and particle size changes occurred to TiO{sub 2} during deposition. It was found that the cold-sprayed TiO{sub 2} film was active for photodegradation of acetaldehyde.
The cephalosporin class antibacterial agent, cefazolin, was intercalated into layered double hydroxides (LDHs) in order to improve the drug efficiency as well as to achieve the controlled release property. Cefazolin molecules were incorporated into LDH through conventional ion exchange reaction. X-raydiffraction pattern analyses confirmed that cefazolin molecules were intercalated between the interlayer spaces of LDH. Fourier-transform infrared spectra and high performance liquid chromatographs clearly showed that the drug molecules were stabilized in LDH lattice through electrostatic interaction and released without any changes in their chemical integrity. Antibacterial activity of the cefazolin-LDH nanohybrid was also examined by an in vitro test, such as the minimal inhibitory concentr...
A 340-watt CO_2 laser is being used to generate PuO_2-UO_2 condensation aerosol from the surface of a Liquid Metal Fast Breeder Reactor (LMFBR) fuel pellet. A wide range of concentrations is achieved by varying the laser power, pulse width, and/or pulse period. The resulting aerosol is composed of branch chain-like aggregates, with the primary particle size ranging between 0.005 and 0.15 #mu#m. X-raydiffraction analyses show that these aerosols condense into a face-centered cubic crystal structure. The activity mean aerodynamic diameter (AMAD), for most power levels, is approximately 0.85 #mu#m with a geometric standard deviation of 1.5.
Silicon layered structures containing porous silicon modified with various thermal treatments and epitaxial layers deposited on porous layers were studied with a number of complementary X-raydiffraction methods using synchrotron source. The methods of characterization included recording of rocking curves for reflections with various asymmetry as well as projection, section and micro-Laue topography. It was found that oxidizing and sintering of porous silicon seriously modified the strains in the porous layer and in some cases even inverting the sense of strain with respect to that in initially formed porous layer. Consequently the deposited epitaxial layer usually was not laterally coherent with the substrate. Some of investigated layers were not stable in time and after few months period exhibited significant lost of coherence of porous skeleton. (author)
To study #beta# #reversible# #omega#-transformation in pseudo-#beta#-titanium alloy VT30, doped by hydrogen, methods of X-raydiffraction and thermodifferential analyses are used. It is established that in the process of heating of the hardened alloy from 0.004-0.1% H first formation and then dissolution of #omega# phase take place. An increase in hydrogen content to 0.1% decreases thermal effect of the processes and does not affect the temperature of #beta# #reversible# #omega#-transformation. Introduction of hydrogen in the concentration of 0.2% and higher suppresses completely #beta# #reversible# #omega# - transformation. A decrease in heating rate displaces #beta# #reversible# #omega#-transformation to lower temperatures.
Intergranular corrosion (IGC) resistance of types 304LN and 316LN stainless steels (SS) thermally aged at 823, 873, and 923 K for various durations was assessed by ASTM A262 practice A test (electrolytic etch test) and electrochemical potentiodynamic reactivation (EPR) test. The results indicated that the type 316LN SS has significantly improved IGC resistance compared to 304LN SS. Based on the results of these tests, time-temperature-sensitization (TTS) diagrams were developed for both alloys. The secondary precipitates formed during thermal aging treatments were electrochemically extracted and analyzed by X-raydiffraction (XRD) to determine the types of precipitates formed during the aging treatments. The results indicated that the precipitates were mostly of M_2_3C_6 carbides.
Intergranular corrosion (IGC) resistance of types 304LN and 316LN stainless steels (SS) thermally aged at 823, 873, and 923 K for various durations was assessed by ASTM A262 practice A test (electrolytic etch test) and electrochemical potentiodynamic reactivation (EPR) test. The results indicated that the type 316LN SS has significantly improved IGC resistance compared to 304LN SS. Based on the results of these tests, time-temperature-sensitization (TTS) diagrams were developed for both alloys. The secondary precipitates formed during thermal aging treatments were electrochemically extracted and analyzed by X-raydiffraction (XRD) to determine the types of precipitates formed during the aging treatments. The results indicated that the precipitates were mostly of M_2_3C_6 carbides.
In situ synthesis of silver chloride (AgCl) nanoparticles was carried out under ambient conditions in nanoporous bacterial cellulose (BC) membranes as nanoreactors. The growth of the nanoparticles was readily obtained by alternating dipping of BC membranes in the solution of silver nitrate or sodium chloride followed by a rinse step. X-raydiffraction (XRD) patterns indicated the existence of AgCl nanoparticles in the BC and scanning electron microscopy (SEM) images showed that the AgCl nanoparticles well dispersed on the surface of BC and penetrated into the BC network. The AgCl nanoparticle-impregnated BC membranes exhibited high hydrophilic ability and strong antimicrobial activity against Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive). The preparative proced...
The ball-milling method was used to produce Mg-50 wt.% ZrFe{sub 1.4}Cr{sub 0.6} composite. The thermodynamic, kinetic, and cycling properties, as well as the resistance to oxidation were examined. This composite possesses excellent kinetic properties, even at moderate temperature. Scanning electron microscopy, energy-dispersive spectrum, transmission electron microscopy and X-raydiffraction were used to characterize the composite before and after hydriding. The fine ZrFe{sub 1.4}Cr{sub 0.6} particles covering Mg particles acting as a ''catalytic film'', a significant amount of imperfections and some alloy powder in the Mg matrix introduced by ball milling all contributed to the enhanced absorption/desorption rate. (orig.)
A series of sputtered tungsten-carbon multilayer structures with periods ranging from 2 to 12 nm in the as-prepared state and after annealing at 500 degrees C for 4 hours has been studied with high resolution transmission electron microscopy. The evolution with annealing of the microstructure of these multilayers depends on their period.As-prepared structures appear predominantly amorphous from TEM imaging and diffraction. Annealing results in crystallization of the W-rich layers into WC in the larger period samples, and less complete or no crystallization in the smaller period samples. X-ray scattering reveals that annealing expands the period in a systematic way. The layers remain remarkably well-defined after annealing under these conditions.
Nd{sub 40}Fe{sub 30}Al{sub 10}Co{sub 15}B{sub 5} alloys were fabricated by high energy ball milling method under various conditions. Microstructure of the alloys was investigated by X-raydiffraction and electron microscopy techniques. Magnetic properties were characterized by hysteresis and thermomagnetic measurements. The high coercive fields up to 2.36 T have been observed on the samples consisting of Nd{sub 2}(Fe,Co,Al){sub 14}B, Nd{sub 6}(Fe,Co,Al){sub 14} and Nd crystallites imbedded in a residual amorphous matrix.
The evolution of intergranular lattice strains in a textured, forged bar (Bar) sample of the #alpha# - #beta# titanium alloy Ti-6Al-4V has been characterised using in situ X-raydiffraction. A two-phase elastic-plastic self-consistent (EPSC) model has been developed to rationalise the results. Of the orientations analysed, it is found that the #left brace#2 0 0#right brace# #beta# orientation is the most compliant and that load partitions to this orientation during plasticity. The results from the bar material have then been used to predict the response of unidirectionally rolled plate (UD) Ti-6Al-4V. It is predicted that the residual lattice strains in the #left brace#101-bar0#right brace# and #left brace#112-bar0#right brace# orientations will be significantly higher in the UD material.
The phase stability of silicides of Ni, Pt and Pd in contact with single crystal or amorphous silicon is examined. The presence of a particular silicide phase is identified by X-raydiffraction, and Rutherford backscattering is used to study composition. It is concluded that Pt or Pd silicides are suitable for Schottky barriers. Layers of silicon can be grown quickly by solid phase epitaxy at temperatures of 300-500C and using an intermediate metal film. Experimental results are reported. Doped layers have been obtained which have electrical characteristics suitable for the junctions in solar cells. The effects of impurities and orientation of the substrate on the growth kinetics are discussed.
We report significant enhancement in superconducting properties of yttrium substituted Ce1-xYxOFFeAs superconductors. The polycrystalline samples were prepared by two step solid state reaction technique. X-raydiffraction confirmed tetragonal ZrCuSiAs structure with decrease in both a and c lattice parameters on increasing yttrium substitution (with fixed F content). With smaller ion Y in place of Ce, the transition temperature increased by 6 K. Yttrium doping also lead to higher critical fields as well as broader magnetization loops, particularly at elevated temperature.
Nanosized CaSnO{sub 3} is synthesized by a hydrothermal process and characterized by X-raydiffraction (XRD), Raman spectroscopy, and scanning electron microscopy (SEM). The SEM observation shows the sample has a porous flowerlike morphology. The electrochemical results exhibit that the stable and reversible capacity of 547 mAh g{sup -1} is obtained after 50 cycles at 60 mA g{sup -1} (0.1 C) and the corresponding charge capacity is determined to be 316 mAh g{sup -1} at the current density of 2.5 C. Cyclic voltammetry and electrochemical impedance spectroscopy data are analyzed to complement the galvanostatic results. The observed excellent performance is attributed to the porous structure and large surface area of flowerlike CaSnO{sub 3}.
Indium sulfide thin films were deposited onto indium-tin-oxide coated glass substrate by electrochemical deposition from an aqueous solution containing In2 (SO4) 3 and Na2S2O3. The deposition conditions were optimized on the basis of data obtained by scanning electron microscope, Auger electron spectroscopy and optical transmission measurements. Furthermore, the photosensitivity of the films was observed by means of photoelectrochemical measurements, which confirmed that the indium sulfide showed n-type conduction. The X-raydiffraction and Raman studies revealed that the as-grown films were amorphous or nanocrystalline in nature and became polycrystalline In2S3 after annealing.
Ferroelectric [Pb_0_._9_2(La_1_-_zSb _z)_0_._0_8][Zr_0_._6_0Ti_0_._4_0]O_3 for z = 0.0, 0.3, 0.6, 0.9 and 1 were prepared from their constituent oxides by a solid state reaction technique. The powders were calcined in the temperature range of 1000 deg. C for 6 h. Phase formation, crystal structure and lattice parameter were investigated by X-raydiffraction (XRD) technique. The compacts were sintered at 1250 deg. C for 2 h and their dielectric, ferroelectric and conductive properties were measured. The ferroelectric behavior of the doped samples was studied from their hysteresis loop.
AISI 5140 steel was plasma nitrided at various gas mixtures of nitrogen, hydrogen, and argon to investigate the actions of hydrogen and argon on plasma nitriding. The structural and mechanical properties of ion-nitrided AISI 5140 steel have been assessed by evaluating composition of phases, surface hardness, compound layer thickness, and case depth by using X-raydiffraction (XRD), microhardness tests, and scanning electron microscopy (SEM). It was found that the growth of compound layer can be controlled and the diffusion improved when the gas mixture includes H_2 gas. Additionally, it was determined that the amount of Ar in dual gas mixture must be at 20% minimum to obtain distinctive surface hardness and compound layer thickness.
Recent research carried out in laboratories showed that Saddle field neutral fast atom beam source is a promising method for nitriding of stainless steel. In the present work, the effect of treatment time on the microstructural and mechanical properties of plasma-nitrided stainless steel sample was investigated by this new method. Plasma nitriding was carried out at 420 deg. C and at a pressure of 0.1 Pa for a time range of 1 to 12 h. SEM-EDX, microhardness tests, optical microscopy and X-raydiffraction (XRD) were used to evaluate the mechanical and structural properties of the nitrided layer. It was found that nitriding time has a pronounced effect on the structural and mechanical properties of low-temperature plasma-nitrided samples and produced a precipitation-free thin hard nitrided layer within a short processing time.
This study describes the effect of treatment of Bis(3-triethoxysilyl propyl)tetrasulfane (silane coupling agent, Si69, TESPT) on in situ sodium activated, organo modified bentonite clay - styrene butadiene rubber (SBR) nanocomposite. transmission electron microscopy and Wide angle X-raydiffraction indicated the intercalation as well as partial exfoliation in both the organoclay and silane treated organoclay compound. It was found that about 5% of silane with respect to clay was the optimum dose for the treatment. Around 15% improvement in tensile and tear strength was observed due to silane treatment. Silane treated organoclay exhibited substantial improvement of the fatigue life, compression set, and rebound property. A detailed study of physical property was carried out. A comparison wi...
The authors present results of grazing incidence X-raydiffraction studies concerning the effect of pH (and thus, of headgroup dissociation) on Langmuir monolayers of fatty acids, in the absence of any divalent cations in the aqueous subphase. An increase in pH transforms the distorted-hexagonal S phase first to the partially disordered Rotator-I phase with less distortion, and then to the completely disordered Rotator-II phase with an undistorted hexagonal structure. The S-Rotator-I and Rotator-I-Rotator-II transitions are pushed to lower temperatures with increase in pH. The fact that the effects of pH increase are almost identical to the effects of increasing temperature indicates the important role of headgroup-headgroup interactions in these monolayer phases.
More than 2,500 Moessbauer spectroscopic studies on minerals have been published since 1960. These papers contain approximately 8,000 sets of Moessbauer mineral data on at least 400 different minerals. This information has been compiled into a database that includes isomer shifts, quadrupole splittings, and magnetic hyperfine interactions at room, liquid nitrogen, and liquid helium temperatures. The database provides a profile of the Moessbauer research performed to date on minerals, including type and locality of minerals investigated, significance of the studies and results, and location of the research facilities. The data and information are available both in printed and magnetic form.With the establishment of this resource, the Moessbauer Effect Data Center has begun a systematic evaluation of the Moessbauer mineral data. It is anticipated that this resource can be used for the identification of minerals as powder X-raydiffraction data ...
The transformation mechanism of hexagonal delta phase from the disordered bcc gamma phase has not been reported before in the Zr-rich U-Zr alloy system. With the help of X-raydiffraction, transmission electron microscopy (TEM) and high-resolution TEM analyses it was shown that the gamma to delta conversion takes place by the lattice collapse mechanism of omega transformation. It was also ascertained that a higher aging temperature or time promotes the growth of all four variants of the delta phase within a parent gamma grain. In addition, ab initio electronic structure calculations showed that the bcc to hexagonal transformation, involving partial ordering of the parent bcc phase followed by (111) plane collapse, is energetically favorable.
The intensity of superstructure reflections and associated diffuse scattering from In_0_._5Ga_0_._5P and In_0_._5Al_0_._5P epitaxic layers grown on (001) GaAs substrates was mapped in reciprocal space. The Warren-Cowley short-range-order parameters were obtained through the usual process for evaluating Fourier coefficients. Varying values for the correlation length in different directions indicate how group III atoms stack up in ordered states. The resultant structure with long-range order confirms the hypothesis made on the basis of electron diffraction and high-resolution transmission electron microscopy studies. (orig.).
The influence of irradiation with 2.6 MeV H and He nuclei on the superconducting properties (critical temperature Tsub(c), critical current Isub(c)) of the intermetallic compound Nb_3Sn was studied. Irradiation led to a significant lowering of Tsub(c), while Isub(c) is increasing with the radiation dose. This is assumed to be due to the formation of active pinning centres in the lattice. There is a fast drop of Isub(c) after a peak value has been reached. Annealing of the samples (600-1,000"0C) led to an almost complete recovery of the initial value of Tsub(c). X-raydiffraction showed that irradiation causes considerable distortions of the lattice while the A15 crystal structure is retained. The causes of the radiation effects related to structural defects are discussed. (GSCH).
In this, the last of a series of three papers, we discuss a method of forming iron phosphate ceramics by a reduction process. We report the formation of iron oxide ceramics by reducing hematite with iron in a phosphoric acid solution. The reaction results in a rapid-setting ceramic (at room temperature) with a compressive strength of 3700 psi and a density of 1.7 g/cm{sup 3}. Although the exact mineral form of the binder is difficult to determine because it is mostly amorphous and hence is not amenable to X-raydiffraction analyses, this material is expected to consist of iron hydrophosphates. The reduction process is very useful in recycling several industrial wastes that are rich in hematite, including iron mine tailings, red mud (a caustic waste from the alumina industry), and machining swarfs. Formation of ceramics with red mud and swarfs is also discussed.
In the present study the optical properties of co-evaporated indium sulfide thin films are investigated. Before being optically characterized, the composition as well as the crystalline properties of the film have been checked with the help of energy dispersive spectroscopy (EDX) and X-Raydiffraction (XRD) analyses. The optical absorption coefficient ? of this indium sulfide film has been deduced from reflectivity R(?) and transmission T(?) measurements. The fit of the curve representing ?(h?) suggests that the ?-In2S3 has an indirect bandgap of 2.01?eV. Density functional theory (DFT) calculations are performed on this indium sulfide compound, using TB-LMTO code. Through these band structure investigations, an indirect bandgap is predicted as observed experimentally. The top of the valen...
The compounds CePdSi_2, CeIrSi_2 and CeRhSn_2 have been synthesized and studied by X-raydiffraction, electrical resistivity and magnetic susceptibility. The magnetic susceptibility of CePdSi_2 exhibits two peaks at 6.8 K and 2.5 K, respectively, indicating two antiferromagnetic phase transitions, while that of CeIrSi_2 shows a broad maximum at 150 K, characteristic of valence fluctuating Ce-compounds. CeRhSn_2 remains paramagnetic down to 5 K. The resistivity of CeIrSi_2 exhibits a T"2 dependence at low temperatures, indicating a Fermi-liquid ground state, while those of CePdSi_2 and CeRhSn_2 shows the presence of Kondo and crystal field effects. (orig.).
The growth of the Pd{sub 2}Si thin fllms on Si(111) substrates has been monitored by an {ital in} {ital situ} x-raydiffraction technique in vacuum and in helium atmosphere from 160 to 250 {degree}C. A familiar parabolic growth rate was found, confirming the diffusion-controlled film growth process. The activation energies were found to be 1.34 and 1.37 eV for the measurements performed in vacuum and helium environment, respectively. Stress relaxation in the growing Pd{sub 2}Si fllm was observed when the reaction temperature exceeds 200 {degree}C. The relaxed films showed a higher degree of texture as evidenced by the rocking curve measurements.
The growth of the Pd{sub 2}Si thin fllms on Si(111) substrates has been monitored by an {ital in} {ital situ} x-raydiffraction technique in vacuum and in helium atmosphere from 160 to 250 {degree}C. A familiar parabolic growth rate was found, confirming the diffusion-controlled film growth process. The activation energies were found to be 1.34 and 1.37 eV for the measurements performed in vacuum and helium environment, respectively. Stress relaxation in the growing Pd{sub 2}Si fllm was observed when the reaction temperature exceeds 200 {degree}C. The relaxed films showed a higher degree of texture as evidenced by the rocking curve measurements.
This paper reports on a series of experiments performed to examine the ability of ion beam assisted thermal deposition to produce good adhesion of Au metallization on GaAs left-angle 100 right-angle substrates. A study of the influence of Ar ion-assisted thermal deposition of the Au films as well as in situ pre-sputtering of the GaAs surface with low-energy Ar ions prior to thermal deposition, shows that strong adhesion can be achieved without resorting to chemical cleaning. The substrate temperature and the relative flux of Ar ions to incident Au atoms were varied in order to correlate these parameters with film adhesion. The interfaces of films processed under these various conditions were examined by XTEM, RBS and XPS. Orientation texture was studied by x-raydiffraction (XRD).
In this study, a novel graphene nanosheets (GNSs) coated solid phase microextraction (SPME) fiber was prepared by immobilizing microwave synthesized GNSs on a stainless steel wire. Microwave synthesized GNSs were verified by X-raydiffraction, field emission-scanning electron microscopy (FE-SEM) and transmission electron microscope (TEM). GNS-SPME fiber was characterized using FE-SEM and the results showed the GNS coating was homogeneous, porous, and highly adherent to the surface of the stainless steel fiber. The performance and feasibility of the GNS-SPME fiber was evaluated under one-step microwave assisted (MA) headspace (HS) SPME followed by gas chromatography with electron capture detection for five organochlorine pesticides (OCPs) in aqueous samples. Parameters influencing the extra...
A novel liquid phase alkylation of aniline with methanol over Zn/Cu salts modified kaolin assisted with a pair of porous carbon electrode in slurry-bed reactor under constant current intensity, room temperature and atmospheric pressure was reported. The Zn/Cu salts modified kaolin catalysts were synthesized and characterized by infrared spectrometer (IR), powder X-raydiffraction (XRD) and scanning electron microscopy (SEM), which showed that the transition metals were completely supported on kaolins structure and formed a pored one. The effect parameters, such as initial pH, electrolysis time, metal ratio with kaolin and salts composition in this electrochemical catalytic system, were studied. The procedure was inspected by ultraviolet-visible spectrum (UV-vis), and the product distributi...